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Sample records for 1h 2h 3h

  1. Method for determination of .sup.18 O/.sup.16 O and .sup.2 H/.sup.1 H ratios and .sup.3 H (tritium) concentrations of xylem waters and subsurface waters using time series sampling

    Science.gov (United States)

    Smith, Brian; Menchaca, Leticia

    1999-01-01

    A method for determination of .sup.18 O/.sup.16 O and .sup.2 H/.sup.1 H ratios and .sup.3 H concentrations of xylem and subsurface waters using time series sampling, insulating sampling chambers, and combined .sup.18 O/.sup.16 O, .sup.2 H/.sup.1 H and .sup.3 H concentration data on transpired water. The method involves collecting water samples transpired from living plants and correcting the measured isotopic compositions of oxygen (.sup.18 O/.sup.16 O) and hydrogen (.sup.2 H/.sup.1 H and/or .sup.3 H concentrations) to account for evaporative isotopic fractionation in the leafy material of the plant.

  2. The synthesis of 7-chloro-5-pentadeuteriophenyl-1-methyl-1H-1, 5-benzodiazepine-2,4(3H, 5H)dione (( sup 2 H sub 5 )clobazam)

    Energy Technology Data Exchange (ETDEWEB)

    Borel, A.G.; Abbott, F.S. (British Columbia Univ., Vancouver, BC (Canada). Dept. of Pharmaceutical Sciences)

    1990-07-01

    Pentadeuteriophenyl clobazam was synthesized in essentially quantitative isotopic purity, and characterized by {sup 1}H-NMR and mass spectroscopy. The title compound was found to be >98% pure by HPLC, and its retention time (t{sub R} 6.17 min) was less than that of an authentic clobazam standard (t{sub R} 6.32 min). Of the five steps in the synthesis of clobazam, the most susceptible to deuterium exchange was the nucleophilic substitution of 2,4-dichloronitrobenzene by aniline-d{sub 7} to form N-(5-chloro-2-nitrophenyl)penta-deuteriophenylamine. In this step, the isotopic impurity aniline-2,3,4,5-d{sub 5} introduced protons from nitrogen into the ortho and para positions of the deuteriophenyl ring of N-(5-chloro-2-nitrophenyl)pentadeuteriophenylamine. (author).

  3. /sup 3/H-/sup 1/H shift correlation NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Funke, C.W.; Wagenaars, G.N.; Kaspersen, F.M.

    1986-05-01

    Three two-dimensional /sup 3/H-/sup 1/H chemical shift correlation experiments are described, all using familiar pulse sequences. The experiments reveal the chemical shifts of the /sup 1/H spins which are coupled scalarly to a /sup 3/H spin and, thus, assist in the unambiguous location of this /sup 3/H spin within the molecule. The limitations for molecules involving a /sup 3/H spin which is coupled differently to various /sup 1/H spins are indicated. In practice, the detection limit is of the order of 100 MBq per /sup 3/H-labelling site.

  4. Aminosilanes derived from 1H-benzimidazole-2(3H)-thione

    Energy Technology Data Exchange (ETDEWEB)

    Palomo-Molina, Juliana [Facultad de Ciencias Químicas, Universidad de Colima, Carretera Coquimatlán-Colima, Coquimatlán Colima 28400 (Mexico); García-Báez, Efrén V. [Unidad Profesional Interdisciplinaria de Biotecnología, Instituto Politécnico Nacional, Avenida Acueducto s/n, Barrio La Laguna Ticomán, México DF 07340 (Mexico); Contreras, Rosalinda [Departamento de Química, Centro de Investigación y de Estudios Avanzados del IPN, Apartado Postal 14-740, México DF 07000 (Mexico); Barrio La Laguna Ticomán, México DF 07340 (Mexico); Pineda-Urbina, Kayim; Ramos-Organillo, Angel, E-mail: aaramos@ucol.mx [Facultad de Ciencias Químicas, Universidad de Colima, Carretera Coquimatlán-Colima, Coquimatlán Colima 28400 (Mexico)

    2015-08-12

    In two trimethylsilyl-substituted 1H-benzimidazole-2(3H)-thiones, noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe{sub 3} groups form helicoidal arrangements in one, and dimerization results in the formation of R{sub s} {sup 2}(8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings, in the second compound. Two new molecular structures, namely 1,3-bis(trimethylsilyl)-1H-benzimidazole-2(3H)-thione, C{sub 13}H{sub 22}N{sub 2}SSi{sub 2}, (2), and 1-trimethylsilyl-1H-benzimidazole-2(3H)-thione, C{sub 10}H{sub 14}N{sub 2}SSi, (3), are reported. Both systems were derived from 1H-benzimidazole-2(3H)-thione. Noncovalent C—H⋯π interactions between the centroid of the benzmidazole system and the SiMe{sub 3} groups form helicoidal arrangements in (2). Dimerization of (3) results in the formation of R{sub 2}{sup 2}(8) rings via N—H⋯S interactions, along with parallel π–π interactions between imidazole and benzene rings.

  5. New Determination of the 2H(d,p)3H and 2H(d,n)3He Reaction Rates at Astrophysical Energies

    Science.gov (United States)

    Tumino, A.; Spartà, R.; Spitaleri, C.; Mukhamedzhanov, A. M.; Typel, S.; Pizzone, R. G.; Tognelli, E.; Degl'Innocenti, S.; Burjan, V.; Kroha, V.; Hons, Z.; La Cognata, M.; Lamia, L.; Mrazek, J.; Piskor, S.; Prada Moroni, P. G.; Rapisarda, G. G.; Romano, S.; Sergi, M. L.

    2014-04-01

    The cross sections of the 2H(d,p)3H and 2H(d,n)3He reactions have been measured via the Trojan Horse method applied to the quasi-free 2H(3He,p 3H)1H and 2H(3He,n 3He)1H processes at 18 MeV off the proton in 3He. For the first time, the bare nucleus S(E) factors have been determined from 1.5 MeV, across the relevant region for standard Big Bang nucleosynthesis, down to the thermal energies of deuterium burning in the pre-main-sequence (PMS) phase of stellar evolution, as well as of future fusion reactors. Both the energy dependence and the absolute value of the S(E) factors deviate by more than 15% from the available direct data and existing fitting curves, with substantial variations in the electron screening by more than 50%. As a consequence, the reaction rates for astrophysics experience relevant changes, with a maximum increase of up to 20% at the temperatures of the PMS phase. From a recent primordial abundance sensitivity study, it turns out that the 2H(d,n)3He reaction is quite influential on 7Li, and the present change in the reaction rate leads to a decrease in its abundance by up to 10%. The present reaction rates have also been included in an updated version of the FRANEC evolutionary code to analyze their influence on the central deuterium abundance in PMS stars with different masses. The largest variation of about 10%-15% pertains to young stars (=1 M ⊙.

  6. Study of the tau- -> 3h- 2h+ nu-tau Decay

    CERN Document Server

    Aubert, B; Boutigny, D; Couderc, F; Gaillard, J M; Hicheur, A; Karyotakis, Yu; Lees, J P; Tisserand, V; Zghiche, A; Palano, A; Pompili, A; Chen, J C; Qi, N D; Rong, G; Wang, P; Zhu, Y S; Eigen, G; Ofte, I; Stugu, B; Abrams, G S; Borgland, A W; Breon, A B; Brown, D N; Button-Shafer, J; Cahn, R N; Charles, E; Day, C T; Gill, M S; Gritsan, A V; Groysman, Y; Jacobsen, R G; Kadel, R W; Kadyk, J; Kerth, L T; Kolomensky, Yu G; Kukartsev, G; Lynch, G; Mir, L M; Oddone, P J; Orimoto, T J; Pripstein, M; Roe, N A; Ronan, Michael T; Shelkov, V G; Wenzel, W A; Barrett, M; Ford, K E; Harrison, T J; Hart, A J; Hawkes, C M; Morgan, S E; Watson, A T; Fritsch, M; Goetzen, K; Held, T; Koch, H; Lewandowski, B; Pelizaeus, M; Steinke, M; Boyd, J T; Chevalier, N; Cottingham, W N; Kelly, M P; Latham, T E; Wilson, F F; Çuhadar-Dönszelmann, T; Hearty, C; Knecht, N S; Mattison, T S; McKenna, J A; Thiessen, D; Khan, A; Kyberd, P; Teodorescu, L; Blinov, A E; Blinov, V E; Druzhinin, V P; Golubev, V B; Ivanchenko, V N; Kravchenko, E A; Onuchin, A P; Serednyakov, S I; Skovpen, Yu I; Solodov, E P; Yushkov, A N; Best, D; Bruinsma, M; Chao, M; Eschrich, I; Kirkby, D; Lankford, A J; Mandelkern, M A; Mommsen, R K; Röthel, W; Stoker, D P; Buchanan, C; Hartfiel, B L; Foulkes, S D; Gary, J W; Shen, B C; Wang, K; Del Re, D; Hadavand, H K; Hill, E J; MacFarlane, D B; Paar, H P; Rahatlou, S; Sharma, V; Berryhill, J W; Campagnari, C; Dahmes, B; Long, O; Lu, A; Mazur, M A; Richman, J D; Verkerke, W; Beck, T W; Eisner, A M; Heusch, C A; Kroseberg, J; Lockman, W S; Nesom, G; Schalk, T; Schumm, B A; Seiden, A; Spradlin, P; Williams, D C; Wilson, M G; Albert, J; Chen, E; Dubois-Felsmann, G P; Dvoretskii, A; Hitlin, D G; Narsky, I; Piatenko, T; Porter, F C; Ryd, A; Samuel, A; Yang, S; Jayatilleke, S M; Mancinelli, G; Meadows, B T; Sokoloff, M D; Abe, T; Blanc, F; Bloom, P; Chen, S; Ford, W T; Nauenberg, U; Olivas, A; Rankin, P; Smith, J G; Zhang, J; Zhang, L; Chen, A; Harton, J L; Soffer, A; Toki, W H; Wilson, R J; Zeng, Q; Altenburg, D; Brandt, T; Brose, J; Dickopp, M; Feltresi, E; Hauke, A; Lacker, H M; Müller-Pfefferkorn, R; Nogowski, R; Otto, S; Petzold, A; Schubert, J; Schubert, Klaus R; Schwierz, R; Spaan, B; Sundermann, J E; Bernard, D; Bonneaud, G R; Brochard, F; Grenier, P; Schrenk, S; Thiebaux, C; Vasileiadis, G; Verderi, M; Bard, D J; Clark, P J; Lavin, D; Muheim, F; Playfer, S; Xie, Y; Andreotti, M; Azzolini, V; Bettoni, D; Bozzi, C; Calabrese, R; Cibinetto, G; Luppi, E; Negrini, M; Piemontese, L; Sarti, A; Treadwell, E; Anulli, F; Baldini-Ferroli, R; Calcaterra, A; De Sangro, R; Finocchiaro, G; Patteri, P; Peruzzi, I M; Piccolo, M; Zallo, A; Buzzo, A; Capra, R; Contri, R; Crosetti, G; Lo Vetere, M; Macri, M; Monge, M R; Passaggio, S; Patrignani, C; Robutti, E; Santroni, A; Tosi, S; Bailey, S; Brandenburg, G; Chaisanguanthum, K S; Morii, M; Won, E; Dubitzky, R S; Langenegger, U; Bhimji, W; Bowerman, D A; Dauncey, P D; Egede, U; Gaillard, J R; Morton, G W; Nash, J A; Nikolich, M B; Taylor, G P; Charles, M J; Grenier, G J; Mallik, U; Cochran, J; Crawley, H B; Lamsa, J; Meyer, W T; Prell, S; Rosenberg, E I; Rubin, A E; Yi, J; Biasini, M; Covarelli, R; Pioppi, M; Davier, M; Giroux, X; Grosdidier, G; Höcker, A; Laplace, S; Le Diberder, F R; Lepeltier, V; Lutz, A M; Petersen, T C; Plaszczynski, S; Schune, M H; Tantot, L; Wormser, G; Cheng, C H; Lange, D J; Simani, M C; Wright, D M; Bevan, A J; Chavez, C A; Coleman, J P; Forster, I J; Fry, J R; Gabathuler, Erwin; Gamet, R; Hutchcroft, D E; Parry, R J; Payne, D J; Sloane, R J; Touramanis, C; Back, J J; Harrison, P F; Mohanty, G B; Cowan, G; Flack, R L; Flächer, H U; Green, M G; Jackson, P S; McMahon, T R; Ricciardi, S; Salvatore, F; Winter, M A; Brown, D; Davis, C L; Allison, J; Barlow, N R; Barlow, R J; Hart, P A; Hodgkinson, M C; Lafferty, G D; Lyon, A J; Williams, J C; Farbin, A; Hulsbergen, W D; Jawahery, A; Kovalskyi, D; Lae, C K; Lillard, V; Roberts, D A; Blaylock, G; Dallapiccola, C; Flood, K T; Hertzbach, S S; Kofler, R; Koptchev, V B; Moore, T B; Saremi, S; Stängle, H; Willocq, S; Cowan, R; Sciolla, G; Sekula, S J; Taylor, F; Yamamoto, R K; Mangeol, D J J; Patel, P M; Robertson, S H; Lazzaro, A; Lombardo, V; Palombo, F; Bauer, J M; Cremaldi, L M; Eschenburg, V; Godang, R; Kroeger, R; Reidy, J; Sanders, D A; Summers, D J; Zhao, H W; Brunet, S; Côté, D; Taras, P; Nicholson, H; Cavallo, N; Lista, L; Monorchio, D; Paolucci, P; Piccolo, D; Sciacca, C; Baak, M; Bulten, H; Raven, G; Snoek, H L; Wilden, L; Jessop, C P; LoSecco, J M; Allmendinger, T; Gan, K K; Honscheid, K; Hufnagel, D; Kagan, H; Kass, R; Pulliam, T; Rahimi, A M; Ter-Antonian, R; Wong, Q K; Brau, J E; Frey, R; Igonkina, O; Potter, C T; Sinev, N B; Strom, D; Torrence, E; Colecchia, F; Dorigo, A; Galeazzi, F; Margoni, M; Morandin, M; Posocco, M; Rotondo, M; Simonetto, F; Stroili, R; Tiozzo, G; Voci, C; Benayoun, M; Briand, H; Chauveau, J; David, P; La Vaissière, C de; Del Buono, L; Hamon, O; John, M J J; Leruste, P; Malcles, J; Ocariz, J; Pivk, M; Roos, L; T'Jampens, S; Therin, G; Manfredi, P F; Re, V; Behera, P K; Gladney, L; Guo, Q H; Panetta, J; Angelini, C; Batignani, G; Bettarini, S; Bondioli, M; Bucci, F; Calderini, G; Carpinelli, M; Forti, F; Giorgi, M A; Lusiani, A; Marchiori, G; Martínez-Vidal, F; Neri, N; Paoloni, E; Rama, M; Rizzo, G; Sandrelli, F; Walsh, J; Haire, M; Judd, D; Paick, K; Wagoner, D E; Danielson, N; Elmer, P; Lau, Y P; Lü, C; Miftakov, V; Olsen, J; Smith, A J S; Telnov, A V; Bellini, F; Cavoto, G; Faccini, R; Ferrarotto, F; Ferroni, F; Gaspero, M; Li Gioi, L; Mazzoni, M A; Morganti, S; Pierini, M; Piredda, G; Safai-Tehrani, F; Voena, C; Christ, S; Wagner, G; Waldi, R; Adye, T; De Groot, N; Franek, B J; Geddes, N I; Gopal, G P; Olaiya, E O; Aleksan, Roy; Emery, S; Gaidot, A; Ganzhur, S F; Giraud, P F; Hamel de Monchenault, G; Kozanecki, Witold; Legendre, M; London, G W; Mayer, B; Schott, G; Vasseur, G; Yéche, C; Zito, M; Purohit, M V; Weidemann, A W; Wilson, J R; Yumiceva, F X; Aston, D; Bartoldus, R; Berger, N; Boyarski, A M; Buchmüller, O L; Claus, R; Convery, M R; Cristinziani, M; De Nardo, Gallieno; Dong, D; Dorfan, J; Dujmic, D; Dunwoodie, W M; Elsen, E E; Fan, S; Field, R C; Glanzman, T; Gowdy, S J; Hadig, T; Halyo, V; Hast, C; Hrynóva, T; Innes, W R; Kelsey, M H; Kim, P; Kocian, M L; Leith, D W G S; Libby, J; Luitz, S; Lüth, V; Lynch, H L; Marsiske, H; Messner, R; Müller, D R; O'Grady, C P; Ozcan, V E; Perazzo, A; Perl, M; Petrak, S; Ratcliff, B N; Roodman, A; Salnikov, A A; Schindler, R H; Schwiening, J; Simi, G; Snyder, A; Soha, A; Stelzer, J; Su, D; Sullivan, M K; Vavra, J; Wagner, S R; Weaver, M; Weinstein, A J R; Wisniewski, W J; Wittgen, M; Wright, D H; Yarritu, A K; Young, C C; Burchat, Patricia R; Edwards, A J; Meyer, T I; Petersen, B A; Roat, C; Ahmed, S; Alam, M S; Ernst, J A; Saeed, M A; Saleem, M; Wappler, F R; Bugg, W; Krishnamurthy, M; Spanier, S M; Eckmann, R; Kim, H; Ritchie, J L; Satpathy, A; Schwitters, R F; Izen, J M; Kitayama, I; Lou, X C; Ye, S; Bianchi, F; Bóna, M; Gallo, F; Gamba, D; Bosisio, L; Cartaro, C; Cossutti, F; Della Ricca, G; Dittongo, S; Grancagnolo, S; Lanceri, L; Poropat, P; Vuagnin, G; Panvini, R S; Banerjee, Sw; Brown, C M; Fortin, D; Jackson, P D; Kowalewski, R V; Roney, J M; Sobie, R J; Band, H R; Cheng, B; Dasu, S; Datta, M; Eichenbaum, A M; Graham, M; Hollar, J J; Johnson, J R; Kutter, P E; Li, H; Liu, R; Mihályi, A; Mohapatra, A K; Pan, Y; Prepost, R; Tan, P; Von Wimmersperg-Töller, J H; Wu, J; Wu, S L; Yu, Z; Greene, M G; Neal, H

    2004-01-01

    A preliminary measurement of the branching fraction of the tau- -> 3h-2h+nu decay (h= pi, K$) with the BaBar detector is found to be {8.52 +/- 0.09 +/- 0.40} x 10E-4, where the first error is statistical and the second is systematic. The data show evidence that the rho resonance plays a strong role in the decay of the tau lepton to five charged hadrons.

  7. Electrowetting Performances of Novel Fluorinated Polymer Dielectric Layer Based on Poly(1H,1H,2H,2H-perfluoroctylmethacrylate Nanoemulsion

    Directory of Open Access Journals (Sweden)

    Jiaxin Hou

    2017-06-01

    Full Text Available In electrowetting devices, hydrophobic insulating layer, namely dielectric layer, is capable of reversibly switching surface wettability through applied electric field. It is critically important but limited by material defects in dielectricity, reversibility, film forming, adhesiveness, price and so on. To solve this key problem, we introduced a novel fluorinated polyacrylate—poly(1H,1H,2H,2H-perfluoroctylmethacrylate (PFMA to construct micron/submicron-scale dielectric layer via facile spray coating of nanoemulsion for replacing the most common Teflon AF series. All the results illustrated that, continuous and dense PFMA film with surface relief less than 20 nm was one-step fabricated at 110 °C, and exhibited much higher static water contact angle of 124°, contact angle variation of 42°, dielectric constant of about 2.6, and breakdown voltage of 210 V than Teflon AF 1600. Particularly, soft and highly compatible polyacrylate mainchain assigned five times much better adhesiveness than common adhesive tape, to PFMA layer. As a promising option, PFMA dielectric layer may further facilitate tremendous development of electrowetting performances and applications.

  8. Characterization Results for the 2014 HTF 3H & 2H Evaporator Overhead Samples

    Energy Technology Data Exchange (ETDEWEB)

    Washington, A. [Savannah River Site (SRS), Aiken, SC (United States)

    2015-05-11

    This report tabulates the radiochemical analysis of the 3H and 2H evaporator overhead samples for 137Cs, 90Sr, and 129I to meet the requirements in the Effluent Treatment Project (ETP) Waste Acceptance Criteria (WAC) (rev. 6). This report identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. All data was found to be within the ETP WAC (rev. 6) specification for the Waste Water Collection Tanks (WWCT).

  9. Study of the tau- --> 3h-2h+nu Decay

    CERN Document Server

    Aubert, B; Boutigny, D; Couderc, F; Karyotakis, Yu; Lees, J P; Poireau, V; Tisserand, V; Zghiche, A; Graugès-Pous, E; Palano, A; Pompili, A; Chen, J C; Qi, N D; Rong, G; Wang, P; Zhu, Y S; Eigen, G; Ofte, I; Stugu, B; Abrams, G S; Borgland, A W; Breon, A B; Brown, D N; Button-Shafer, J; Cahn, R N; Charles, E; Day, C T; Gill, M S; Gritsan, A V; Groysman, Y; Jacobsen, R G; Kadel, R W; Kadyk, J; Kerth, L T; Kolomensky, Yu G; Kukartsev, G; Lynch, G; Mir, L M; Oddone, P J; Orimoto, T J; Pripstein, M; Roe, N A; Ronan, Michael T; Wenzel, W A; Barrett, M; Ford, K E; Harrison, T J; Hart, A J; Hawkes, C M; Morgan, S E; Watson, A T; Fritsch, M; Goetzen, K; Held, T; Koch, H; Lewandowski, B; Pelizaeus, M; Schröder, T; Steinke, M; Boyd, J T; Chevalier, N; Cottingham, W N; Kelly, M P; Latham, T E; Wilson, F F; Çuhadar-Dönszelmann, T; Hearty, C; Knecht, N S; Mattison, T S; McKenna, J A; Thiessen, D; Khan, A; Kyberd, P; Teodorescu, L; Blinov, A E; Blinov, V E; Druzhinin, V P; Golubev, V B; Ivanchenko, V N; Kravchenko, E A; Onuchin, A P; Serednyakov, S I; Skovpen, Yu I; Solodov, E P; Yushkov, A N; Best, D; Bruinsma, M; Chao, M; Eschrich, I; Kirkby, D; Lankford, A J; Mandelkern, M A; Mommsen, R K; Röthel, W; Stoker, D P; Buchanan, C; Hartfiel, B L; Weinstein, A J R; Foulkes, S D; Gary, J W; Long, O; Shen, B C; Wang, K; Del Re, D; Hadavand, H K; Hill, E J; MacFarlane, D B; Paar, H P; Rahatlou, S; Sharma, V; Berryhill, J W; Campagnari, C; Cunha, A; Dahmes, B; Hong, T M; Lu, A; Mazur, M A; Richman, J D; Verkerke, W; Beck, T W; Eisner, A M; Heusch, C A; Kroseberg, J; Lockman, W S; Nesom, G; Schalk, T; Schumm, B A; Seiden, A; Spradlin, P; Williams, D C; Wilson, M G; Albert, J; Chen, E; Dubois-Felsmann, G P; Dvoretskii, A; Hitlin, D G; Narsky, I; Piatenko, T; Porter, F C; Ryd, A; Samuel, A; Yang, S; Jayatilleke, S M; Mancinelli, G; Meadows, B T; Sokoloff, M D; Blanc, F; Bloom, P; Chen, S; Ford, W T; Nauenberg, U; Olivas, A; Rankin, P; Ruddick, W O; Smith, J G; Ulmer, K A; Zhang, J; Zhang, L; Chen, A; Eckhart, E A; Harton, J L; Soffer, A; Toki, W H; Wilson, R J; Zeng, Q; Spaan, B; Altenburg, D; Brandt, T; Brose, J; Dickopp, M; Feltresi, E; Hauke, A; Lacker, H M; Nogowski, R; Otto, S; Petzold, A; Schubert, J; Schubert, K R; Schwierz, R; Sundermann, J E; Bernard, D; Bonneaud, G R; Grenier, P; Schrenk, S; Thiebaux, C; Vasileiadis, G; Verderi, M; Bard, D J; Clark, P J; Muheim, F; Playfer, S; Xie, Y; Andreotti, M; Azzolini, V; Bettoni, D; Bozzi, C; Calabrese, R; Cibinetto, G; Luppi, E; Negrini, M; Piemontese, L; Sarti, A; Anulli, F; Baldini-Ferroli, R; Calcaterra, A; De Sangro, R; Finocchiaro, G; Patteri, P; Peruzzi, I M; Piccolo, M; Zallo, A; Buzzo, A; Capra, R; Contri, R; Crosetti, G; Lo Vetere, M; Macri, M; Monge, M R; Passaggio, S; Patrignani, C; Robutti, E; Santroni, A; Tosi, S; Bailey, S; Brandenburg, G; Chaisanguanthum, K S; Morii, M; Won, E; Dubitzky, R S; Langenegger, U; Marks, J; Uwer, U; Bhimji, W; Bowerman, D A; Dauncey, P D; Egede, U; Gaillard, J R; Morton, G W; Nash, J A; Nikolich, M B; Taylor, G P; Charles, M J; Grenier, G J; Mallik, U; Cochran, J; Crawley, H B; Lamsa, J; Meyer, W T; Prell, S; Rosenberg, E I; Rubin, A E; Yi, J; Arnaud, N; Davier, M; Giroux, X; Grosdidier, G; Höcker, A; Le Diberder, F R; Lepeltier, V; Lutz, A M; Petersen, T C; Plaszczynski, S; Schune, M H; Wormser, G; Cheng, C H; Lange, D J; Simani, M C; Wright, D M; Bevan, A J; Chavez, C A; Coleman, J P; Forster, I J; Fry, J R; Gabathuler, Erwin; Gamet, R; Hutchcroft, D E; Parry, R J; Payne, D J; Touramanis, C; Cormack, C M; Di Lodovico, F; Brown, C L; Cowan, G; Flack, R L; Flächer, H U; Green, M G; Jackson, P S; McMahon, T R; Ricciardi, S; Salvatore, F; Winter, M A; Brown, D; Davis, C L; Allison, J; Barlow, N R; Barlow, R J; Hodgkinson, M C; Lafferty, G D; Williams, J C; Chen, C; Farbin, A; Hulsbergen, W D; Jawahery, A; Kovalskyi, D; Lae, C K; Lillard, V; Roberts, D A; Blaylock, G; Dallapiccola, C; Hertzbach, S S; Kofler, R; Koptchev, V B; Moore, T B; Saremi, S; Stängle, H; Willocq, S; Cowan, R; Koeneke, K; Sciolla, G; Sekula, S J; Taylor, F; Yamamoto, R K; Patel, P M; Robertson, S H; Lazzaro, A; Lombardo, V; Palombo, F; Bauer, J M; Cremaldi, L M; Eschenburg, V; Godang, R; Kroeger, R; Reidy, J; Sanders, D A; Summers, D J; Zhao, H W; Brunet, S; Côté, D; Taras, P; Nicholson, H; Cavallo, N; Fabozzi, F; Gatto, C; Lista, L; Monorchio, D; Paolucci, P; Piccolo, D; Sciacca, C; Baak, M; Bulten, H; Raven, G; Snoek, H L; Wilden, L; Jessop, C P; LoSecco, J M; Allmendinger, T; Benelli, G; Gan, K K; Honscheid, K; Hufnagel, D; Kagan, H; Kass, R; Pulliam, T; Rahimi, A M; Ter-Antonian, R; Wong, Q K; Brau, J E; Frey, R; Igonkina, O; Lu, M; Potter, C T; Sinev, N B; Strom, D; Torrence, E; Colecchia, F; Dorigo, A; Galeazzi, F; Margoni, M; Morandin, M; Posocco, M; Rotondo, M; Simonetto, F; Stroili, R; Voci, C; Benayoun, M; Briand, H; Chauveau, J; David, P; La Vaissière, C de; Del Buono, L; Hamon, O; John, M J J; Leruste, P; Malcles, J; Ocariz, J; Roos, L; Therin, G; Behera, P K; Gladney, L; Guo, Q H; Panetta, J; Biasini, M; Covarelli, R; Pioppi, M; Angelini, C; Batignani, G; Bettarini, S; Bondioli, M; Bucci, F; Calderini, G; Carpinelli, M; Forti, F; Giorgi, M A; Lusiani, A; Marchiori, G; Morganti, M; Neri, N; Paoloni, E; Rama, M; Rizzo, G; Simi, G; Walsh, J; Haire, M; Judd, D; Paick, K; Wagoner, D E; Danielson, N; Elmer, P; Lau, Y P; Lü, C; Miftakov, V; Olsen, J; Smith, A J S; Telnov, A V; Bellini, F; Cavoto, G; D'Orazio, A; Di Marco, E; Faccini, R; Ferrarotto, F; Ferroni, F; Gaspero, M; Li Gioi, L; Mazzoni, M A; Morganti, S; Pierini, M; Piredda, G; Polci, F; Safai-Tehrani, F; Voena, C; Christ, S; Schröder, H; Wagner, G; Waldi, R; Adye, T; De Groot, N; Franek, B J; Gopal, G P; Olaiya, E O; Aleksan, Roy; Emery, S; Gaidot, A; Ganzhur, S F; Giraud, P F; Hamel de Monchenault, G; Kozanecki, Witold; Legendre, M; London, G W; Mayer, B; Schott, G; Vasseur, G; Yéche, C; Zito, M; Purohit, M V; Weidemann, A W; Wilson, J R; Yumiceva, F X; Abe, T; Allen, M; Aston, D; Bartoldus, R; Berger, N; Boyarski, A M; Buchmüller, O L; Claus, R; Convery, M R; Cristinziani, M; De Nardo, Gallieno; Dingfelder, J C; Dong, D; Dorfan, J; Dujmic, D; Dunwoodie, W M; Fan, S; Field, R C; Glanzman, T; Gowdy, S J; Hadig, T; Halyo, V; Hast, C; Hrynóva, T; Innes, W R; Kelsey, M H; Kim, P; Kocian, M L; Leith, D W G S; Libby, J; Luitz, S; Lüth, V; Lynch, H L; Marsiske, H; Messner, R; Müller, D R; O'Grady, C P; Ozcan, V E; Perazzo, A; Perl, M; Ratcliff, B N; Roodman, A; Salnikov, A A; Schindler, R H; Schwiening, J; Snyder, A; Soha, A; Stelzer, J; Strube, J; Su, D; Sullivan, M K; Thompson, J; Vavra, J; Wagner, S R; Weaver, M; Wisniewski, W J; Wittgen, M; Wright, D H; Yarritu, A K; Young, C C; Burchat, Patricia R; Edwards, A J; Majewski, S A; Petersen, B A; Roat, C; Ahmed, M; Ahmed, S; Alam, M S; Ernst, J A; Saeed, M A; Saleem, M; Wappler, F R; Bugg, W; Krishnamurthy, M; Spanier, S M; Eckmann, R; Kim, H; Ritchie, J L; Satpathy, A; Schwitters, R F; Izen, J M; Kitayama, I; Lou, X C; Ye, S; Bianchi, F; Bóna, M; Gallo, F; Gamba, D; Bosisio, L; Cartaro, C; Cossutti, F; Della Ricca, G; Dittongo, S; Grancagnolo, S; Lanceri, L; Poropat, P; Vitale, L; Vuagnin, G; Martínez-Vidal, F; Panvini, R S; Banerjee, S; Bhuyan, B; Brown, C M; Fortin, D; Jackson, P D; Kowalewski, R V; Roney, J M; Sobie, R J; Back, J J; Harrison, P F; Mohanty, G B; Band, H R; Chen, X; Cheng, B; Dasu, S; Datta, M; Eichenbaum, A M; Flood, K T; Graham, M; Hollar, J J; Johnson, J R; Kutter, P E; Li, H; Liu, R; Mihályi, A; Pan, Y; Prepost, R; Tan, P; Von Wimmersperg-Töller, J H; Wu, J; Wu, S L; Yu, Z; Greene, M G; Neal, H

    2005-01-01

    The branching fraction of the tau- --> 3h- 2h+ nu decay (h= pi, kaon) is measured with the BaBar detector to be (8.56 +/- 0.05 +/- 0.42)E-04 where the first error is statistical and the second systematic. The observed structure of this decay is significantly different from the phase space prediction, with the rho resonance playing a strong role. The decay tau- --> f1 pi nu with the f1 meson decaying to four charged pions, is observed and the branching fraction is measured to be (3.9 +/- 0.7 +/- 0.5)E-04.

  10. Investigation of Coating Performance of UV-Curable Hybrid Polymers Containing 1H,1H,2H,2H-Perfluorooctyltriethoxysilane Coated on Aluminum Substrates

    Directory of Open Access Journals (Sweden)

    Mustafa Çakır

    2017-03-01

    Full Text Available This study describes preparation and characterization of fluorine-containing organic-inorganic hybrid coatings. The organic part consists of bisphenol-A glycerolate (1 glycerol/phenol diacrylate resin and 1,6-hexanediol diacrylate reactive diluent. The inorganically rich part comprises trimethoxysilane-terminated urethane, 1H,1H,2H,2H-perfluorooctyltriethoxysilane, 3-(trimethoxysilyl propyl methacrylate and sol–gel precursors that are products of hydrolysis and condensation reactions. Bisphenol-A glycerolate (1 glycerol/phenol diacrylate resin was added to the inorganic part in predetermined amounts. The resultant mixture was utilized in the preparation of free films as well as coatings on aluminum substrates. Thermal and mechanical tests such as DSC, thermo-gravimetric analysis (TGA, and tensile and shore D hardness tests were performed on free films. Water contact angle, gloss, Taber abrasion test, cross-cut and tubular impact tests were conducted on the coated samples. SEM examination and EDS analysis was performed on the fractured surfaces of free films. The hybrid coatings on the aluminum sheets gave rise to properties such as moderately glossed surface; low wear rate and hydrophobicity. Tensile strength of free films increased with up to 10% inorganic content in the hybrid structure and this increase was approximately three times that of the control sample. As expected; the % strain value decreased by 17.3 with the increase in inorganic content and elastic modulus values increased by a factor of approximately 6. Resistance to ketone-based solvents was proven and an increase in hardness was observed as the ratio of the inorganic part increased. Samples which contain 10% sol–gel content were observed to provide optimal properties.

  11. NMR resonance splitting of urea in stretched hydrogels: proton exchange and (1)H/(2)H isotopologues.

    Science.gov (United States)

    Kuchel, Philip W; Naumann, Christoph; Chapman, Bogdan E; Shishmarev, Dmitry; Håkansson, Pär; Bacskay, George; Hush, Noel S

    2014-10-01

    Urea at ∼12 M in concentrated gelatin gel, that was stretched, gave (1)H and (2)H NMR spectral splitting patterns that varied in a predictable way with changes in the relative proportions of (1)H2O and (2)H2O in the medium. This required consideration of the combinatorics of the two amide groups in urea that have a total of four protonation/deuteration sites giving rise to 16 different isotopologues, if all the atoms were separately identifiable. The rate constant that characterized the exchange of the protons with water was estimated by back-transformation analysis of 2D-EXSY spectra. There was no (1)H NMR spectral evidence that the chiral gelatin medium had caused in-equivalence in the protons bonded to each amide nitrogen atom. The spectral splitting patterns in (1)H and (2)H NMR spectra were accounted for by intra-molecular scalar and dipolar interactions, and quadrupolar interactions with the electric field gradients of the gelatin matrix, respectively.

  12. (1)H-(2)H cross-polarization NMR in fast spinning solids by adiabatic sweeps.

    Science.gov (United States)

    Wi, Sungsool; Schurko, Robert; Frydman, Lucio

    2017-03-14

    Cross-polarization (CP) experiments employing frequency-swept radiofrequency (rf) pulses have been successfully used in static spin systems for obtaining broadband signal enhancements. These experiments have been recently extended to heteronuclear I, S = spin-1/2 nuclides under magic-angle spinning (MAS), by applying adiabatic inversion pulses along the S (low-γ) channel while simultaneously applying a conventional spin-locking pulse on the I-channel ((1)H). This study explores an extension of this adiabatic frequency sweep concept to quadrupolar nuclei, focusing on CP from (1)H (I = 1/2) to (2)H spins (S = 1) undergoing fast MAS (νr = 60 kHz). A number of new features emerge, including zero- and double-quantum polarization transfer phenomena that depend on the frequency offsets of the swept pulses, the rf pulse powers, and the MAS spinning rate. An additional mechanism found operational in the (1)H-(2)H CP case that was absent in the spin-1/2 counterpart, concerns the onset of a pseudo-static zero-quantum CP mode, driven by a quadrupole-modulated rf/dipolar recoupling term arising under the action of MAS. The best CP conditions found at these fast spinning rates correspond to double-quantum transfers, involving weak (2)H rf field strengths. At these easily attainable (ca. 10 kHz) rf field conditions, adiabatic level-crossings among the {|1⟩,|0⟩,|-1⟩} mS energy levels, which are known to complicate the CP MAS of quadrupolar nuclei, are avoided. Moreover, the CP line shapes generated in this manner are very close to the ideal (2)H MAS spectral line shapes, facilitating the extraction of quadrupolar coupling parameters. All these features were corroborated with experiments on model compounds and justified using numerical simulations and average Hamiltonian theory models. Potential applications of these new phenomena, as well as extensions to higher spins S, are briefly discussed.

  13. Nqrs Data for C3H12INO7 [C3H7NO2·HIO3·2(H2O)] (Subst. No. 0646)

    Science.gov (United States)

    Chihara, H.; Nakamura, N.

    This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C3H12INO7 [C3H7NO2·HIO3·2(H2O)] (Subst. No. 0646)

  14. Inhibition of myeloperoxidase: evaluation of 2H-indazoles and 1H-indazolones.

    Science.gov (United States)

    Roth, Aaron; Ott, Sean; Farber, Kelli M; Palazzo, Teresa A; Conrad, Wayne E; Haddadin, Makhluf J; Tantillo, Dean J; Cross, Carroll E; Eiserich, Jason P; Kurth, Mark J

    2014-11-15

    Myeloperoxidase (MPO) produces hypohalous acids as a key component of the innate immune response; however, release of these acids extracellularly results in inflammatory cell and tissue damage. The two-step, one-pot Davis-Beirut reaction was used to synthesize a library of 2H-indazoles and 1H-indazolones as putative inhibitors of MPO. A structure-activity relationship study was undertaken wherein compounds were evaluated utilizing taurine-chloramine and MPO-mediated H2O2 consumption assays. Docking studies as well as toxicophore and Lipinski analyses were performed. Fourteen compounds were found to be potent inhibitors with IC50 values <1μM, suggesting these compounds could be considered as potential modulators of pro-oxidative tissue injury pertubated by the inflammatory MPO/H2O2/HOCl/HOBr system.

  15. The Cac1 subunit of histone chaperone CAF-1 organizes CAF-1-H3/H4 architecture and tetramerizes histones

    Science.gov (United States)

    Liu, Wallace H; Roemer, Sarah C; Zhou, Yeyun; Shen, Zih-Jie; Dennehey, Briana K; Balsbaugh, Jeremy L; Liddle, Jennifer C; Nemkov, Travis; Ahn, Natalie G; Hansen, Kirk C; Tyler, Jessica K; Churchill, Mair EA

    2016-01-01

    The histone chaperone Chromatin Assembly Factor 1 (CAF-1) deposits tetrameric (H3/H4)2 histones onto newly-synthesized DNA during DNA replication. To understand the mechanism of the tri-subunit CAF-1 complex in this process, we investigated the protein-protein interactions within the CAF-1-H3/H4 architecture using biophysical and biochemical approaches. Hydrogen/deuterium exchange and chemical cross-linking coupled to mass spectrometry reveal interactions that are essential for CAF-1 function in budding yeast, and importantly indicate that the Cac1 subunit functions as a scaffold within the CAF-1-H3/H4 complex. Cac1 alone not only binds H3/H4 with high affinity, but also promotes histone tetramerization independent of the other subunits. Moreover, we identify a minimal region in the C-terminus of Cac1, including the structured winged helix domain and glutamate/aspartate-rich domain, which is sufficient to induce (H3/H4)2 tetramerization. These findings reveal a key role of Cac1 in histone tetramerization, providing a new model for CAF-1-H3/H4 architecture and function during eukaryotic replication. DOI: http://dx.doi.org/10.7554/eLife.18023.001 PMID:27690308

  16. 1H, 1H, 2H, 2H-Perfluoroalkyl-Functionalization of Ni(II), Pd(II) and Pt(II) Mono- and Diphosphine Complexes : minimizing the Electronic Consequences for the Metal Center

    NARCIS (Netherlands)

    Koten, G. van; Wolf, E. de; Mens, A.J.M.; Gijzeman, O.L.J.; Lenthe, J.H. van; Jenneskens, L.W.; Deelman, B.J.

    2003-01-01

    A series of fluorous derivatives of group 10 complexes MCl2(dppe) and [M(dppe)2](BF4)2 (M = Ni, Pd or Pt; dppe = 1,2-bis(diphenylphosphino)ethane) and cis-PtCl2(PPh3)2 was synthesized. The influence of para-(1H,1H,2H,2H-perfluoroalkyl)dimethylsilyl-functionalization of the phosphine phenyl groups of

  17. Hydrochemistry and 18O/16O and 2H/1H Ratios of Ugandan Waters

    Science.gov (United States)

    Gebremichael, M. G.; Jasechko, S.

    2013-12-01

    Today, 70% of the 35 million people living in Uganda have access to an improved water source, ranking Uganda 148 out of 179 nations reporting in 2010 (Millennium Development Goals Indicators). 80% of Ugandans rely on groundwater as their primary drinking water source, collecting at springs or from shallow wells. Similarly, 80% of Ugandans rely upon agriculture - usually rain fed - as their primary income source. Despite lack of access to protected water sources faced by 10 million Ugandans, and the importance of the blue economy to Uganda's continued development, a country-wide investigation of the chemistry and the stable oxygen and hydrogen isotope compositions of waters has yet to be completed. Here we present 250 analyses of 18O/16O, 2H/1H and dissolved ion concentrations of Ugandan lakes, rivers, groundwaters and springs collected during July, 2013. We use the new data to characterize regional scale groundwater recharge sources, advection pathways and interactions with surface waters. Large lakes - Albert, Edward and Victoria - show increases in 18O/16O and 2H/1H ratios consistent with open water evaporation, and are shown to be distinct from nearby groundwaters, suggesting minimal recharge from large lakes to the subsurface. Salinities of eastern Ugandan groundwaters are elevated relative to samples collected from the central and western regions, suggesting that longer groundwater residence times and enhanced water-rock interactions characterize these waters. Springs from western Uganda show a shift in 18O/16O to higher values as a result of hydrothermal water-rock exchanges. Dissolved ion and noble gas concentrations show potential for use in assessing geothermal energy resources, perhaps aiding the Ugandan Ministry for Energy, Minerals and Development to meet their goal of increasing renewable energy from 4% (current) to 61% of total use by 2017 (Nyakabwa-Atwoki, 2013). Millennium Development Goals Indicators. mdgs.un.org/unsd/mdg/data.aspx Nyakabwa

  18. On the formation of cyclopentadiene in the C3H5˙ + C2H2 reaction

    NARCIS (Netherlands)

    Bouwman, J.; Bodi, A.; Oomens, J.; Hemberger, P.

    2015-01-01

    The reaction between the allyl radical (C3H5˙) and acetylene (C2H2) in a heated microtubular reactor has been studied at the VUV beamline of the Swiss Light Source. The reaction products are sampled from the reactor and identified by their photoion mass-selected threshold photoelectron spectra

  19. Ab initio study of {sup 2}H(d,{gamma}){sup 4}He, {sup 2}H(d,p){sup 3}H, and {sup 2}H(d,n){sup 4}He reactions and the tensor force

    Energy Technology Data Exchange (ETDEWEB)

    Arai, K.; Aoyama, S.; Suzuki, Y.; Descouvemont, P.; Baye, D. [Division of General Education, Nagaoka National College of Technology, 888 Nishikatakai, Nagaoka, Niigata, 940-8532 (Japan); Center for Academic Information Service, Niigata University, Niigata 950-2181 (Japan); Department of Physics, Niigata University, Niigata 950-2181, Japan and RIKEN Nishina Center, Wako 351-0198 (Japan); Physique Nucleaire Theorique et Physique Mathematique, C.P.229, Universite Libre de Bruxelles, B 1050 Brussels (Belgium); Physique Quantique, CP165/82, Universite Libre de Bruxelles, B-1050 Brussels (Belgium)

    2012-11-12

    The {sup 2}H(d,p){sup 3}H, {sup 2}H(d,n){sup 3}He, and {sup 2}H(d,{gamma}){sup 4}He reactions at low energies are studied with realistic nucleon-nucleon interactions in an ab initio approach. The obtained astrophysical S-factors are all in very good agreement with experiment. The most important channels for both transfer and radiative capture are all found to dominate thanks to the tensor force.

  20. 1-(4-Methylbenzyl-1H-benzimidazol-2(3H-one

    Directory of Open Access Journals (Sweden)

    Lahcen El Ammari

    2013-01-01

    Full Text Available In the title compound, C15H14N2O, the fused five- and six-membered ring system is essentially planar, the maximum deviation from the mean plane being 0.009 (1 Å. The benzimidazol-2(3H-one residue is nearly perpendicular to the benzyl ring, forming a dihedral angle of 77.41 (6°. In the crystal, inversion dimers are formed by pairs of N—H...O hydrogen bonds; these dimers are linked by weak C—H...O interactions into a two-dimensional array in the (102 plane.

  1. Photoabsorption and photoionization cross sections of NH3, PH3, H2S, C2H2, and C2H4 in the VUV region

    Science.gov (United States)

    Xia, T. J.; Chien, T. S.; Wu, C. Y. Robert; Judge, D. L.

    1991-01-01

    Using synchrotron radiation as a continuum light source, the photoabsorption and photoionization cross sections of NH3, PH3, H2S, C2H2, and C2H4 have been measured from their respective ionization thresholds to 1060 A. The vibrational constants associated with the nu(2) totally symmetric, out-of-plane bending vibration of the ground electronic state of PH3(+) have been obtained. The cross sections and quantum yields for producing neutral products through photoexcitation of these molecules in the given spectral regions have also been determined. In the present work, autoionization processes were found to be less important than dissociation and predissociation processes in NH3, PH3, and C2H4. Several experimental techniques have been employed in order to examine the various possible systematic errors critically.

  2. Trojan Horse particle invariance for 2H(d,p3H reaction: a detailed study

    Directory of Open Access Journals (Sweden)

    Pizzone R.G.

    2014-03-01

    Full Text Available In the last decades the Trojan Horse method has played a crucial role for the measurement of several charged particle induced reactions cross sections of astrophysical interest. To better understand its cornerstones and its applications to physical cases many tests were performed to verify all its properties and the possible future perspectives. The Trojan Horse nucleus invariance for the binary d(d,pt reaction was therefore tested using the quasi free 2H(6Li, pt4He and 2H(3He,ptH reactions after 6Li and 3He break-up, respectively. The astrophysical S(E-factor for the d(d,pt binary process was then extracted in the framework of the Plane Wave Approximation applied to the two different break-up schemes. The obtained results are compared with direct data as well as with previous indirect investigations. The very good agreement confirms the applicability of the plane wave approximation and suggests the independence of binary indirect cross section on the chosen Trojan Horse nucleus also for the present case.

  3. 1H- and 2H-T1 relaxation behavior of the rhodium dihydrogen complex [(triphos)Rh(eta 2-H2)H2]+.

    Science.gov (United States)

    Bakhmutov, V I; Bianchini, C; Peruzzini, M; Vizza, F; Vorontsov, E V

    2000-04-17

    Protonation of the classical trihydride [(triphos)RhH3] (2) at 210 K in either THF or CH2Cl2 by either HBF4.OMe2 or CF3SO2OH gives the nonclassical eta 2-H2 complex [(triphos)Rh(eta 2-H2)H2]+ (1) [triphos = MeC(CH2PPh2)3]. Complex 1 is thermally unstable and highly fluxional in solution. In THF above 230 K, 1 transforms into the solvento dihydride complex [(triphos)Rh(eta 1-THF-d8)H2]+ (5) that, at room temperature, quickly converts to the stable dimer trans-[[(triphos)RhH]2(mu-H)2]2+ (trans-6). In CH2Cl2, 1 is stable up to 240 K. Above this temperature, the eta 2-H2 complex begins to convert into a mixture of trans- and cis-6, which, in turn, transform into the bridging-chloride dimers trans- and cis-[[(triphos)RhH]2(mu-Cl)2]2+ at room temperature. Complex 1 contains a fast-spinning H2 ligand with a T1min of 38.9 ms in CD2Cl2 (220 K, 400 MHz). An NMR analysis of the bis-deuterated isotopomer [(triphos)RhH2D2]+ (1-d2) did not provide a J(HD) value. At 190 K, the perdeuterated isotopomers [(triphos)RhD3] (2-d3) and 1-d4 show T1min values of 16.5 and 32.6 ms (76.753 MHz), respectively, for the rapidly exchanging deuterides. An analogous 2-fold elongation of T1min is also observed on going from [(triphos)IrD3] to [(triphos)Ir(eta 2-D2)D2]+. A rationale for the elongation of T1min in nonclassical polyhydrides is proposed on the basis of both the results obtained and recent literature reports.

  4. A novel synthesis and preliminary in vitro cytotoxic evaluation of dihydropyrimidine-2,4(1H,3H)-dione derivatives

    Indian Academy of Sciences (India)

    V UDAYAKUMAR; J GOWSIKA; A PANDURANGAN

    2017-02-01

    We report the synthesis and characterization of four new compounds: 6-(2-(1H-inden-2-yl) phenyl)-3-(2-morpholinoethyl)dihydropyrimidine-2,4(1H,3H)-dione (13a), 6-(2-(1H-inden-2-yl)phenyl)-3-(2-(pyrrolidin-1-yl)ethyl)dihydropyrimidine-2,4(1H,3H)-dione (13b), 6-(2-(1H-inden-2-yl)phenyl)-3-phenethyldihydropyrimidine-2,4(1H,3H)-dione (13c) and 3-(3-(1H-imidazol-1-yl)propyl)-6-(2-(1H-inden-2-yl)phenyl) dihydropyrimidine-2,4(1H,3H)-dione (13d). A series of dihydropyrimidine-2,4(1H, 3H)-dione moieties was derived from methyl 3-amino-3-(2-chlorophenyl)propanoate precursor in a multi-step synthesis. Acid-aminecoupling of 3-(2-(1H-inden-2-yl)phenyl)-3-((tert-butoxycarbonyl)amino)propanoic acid with a series of amine derivatives under mild reaction conditions led to form the corresponding dihydropyrimidine-2,4(1H, 3H)- dione derivatives via de-Boc and cyclization reaction in modest yield. Spectroscopic (¹H, ¹³C NMR, and Mass) and analytical techniques have been used to identify and confirm the structure of the products.

  5. A NOTE ON THE CONSTRUCTION OF SYMPLECTIC SCHEMES FOR SPLITABLE HAMILTONIAN H = H(1) + H(2) + H(3)

    Institute of Scientific and Technical Information of China (English)

    Yifa Tang

    2002-01-01

    In this note, we will give a proof for the uniqueness of 4th-order time-reversible sym-plectic difference schemes of 13th-fold compositions of phase flows φtH(1), t tφH(2), φH(3) withdifferent temporal parameters for splitable hamiltonian H - H(1) + H(2) + H(3).

  6. Measurement of the 2H(d ,p ) 3H reaction at astrophysical energies via the Trojan-horse method

    Science.gov (United States)

    Li, Chengbo; Wen, Qungang; Fu, Yuanyong; Zhou, Jing; Zhou, Shuhua; Meng, Qiuying; Spitaleri, C.; Tumino, A.; Pizzone, R. G.; Lamia, L.

    2015-08-01

    The study of the 2H(d ,p ) 3H reaction is very important for the nucleosynthesis in both the standard Big Bang and stellar evolution, as well as for the future fusion reactor's planning of energy production. The 2H(d ,p ) 3H bare nucleus astrophysical S (E ) factor has been measured indirectly at energies from about 400 keV down to several keV by means of the Trojan-horse method applied to the quasifree process 2H(6Li ,p t ) 4He induced at a lithium beam energy of 9.5 MeV, which is closer to the zero-quasifree-energy point. An accurate analysis leads to the determination of the Sbare(0 ) =56.7 ±2.0 keV b and of the corresponding electron screening potential Ue=13.2 ±4.3 eV. In addition, this work gives an updated test for the Trojan-horse nucleus invariance by comparing with previous indirect investigations using the 3He=(d +p ) breakup.

  7. Osmium(IV) complexes with 1H- and 2H-indazoles: tautomer identity versus spectroscopic properties and antiproliferative activity.

    Science.gov (United States)

    Büchel, Gabriel E; Stepanenko, Iryna N; Hejl, Michaela; Jakupec, Michael A; Keppler, Bernhard K; Heffeter, Petra; Berger, Walter; Arion, Vladimir B

    2012-08-01

    A one-pot synthesis of osmium(IV) complexes with two different tautomers of indazole, 1H-indazole and 2H-indazole, namely (H(2)ind)[Os(IV)Cl(5)(2H-ind)] (1) and (H(2)ind)[Os(IV)Cl(5)(1H-ind)] (2) is reported. Both compounds have been comprehensively characterized by NMR spectroscopy, ESI (electrospray ionization) mass spectrometry, electronic absorption spectroscopy, IR spectroscopy, cyclic voltammetry and tested for antiproliferative activity in vitro in three human cancer cell lines, CH1 (ovarian carcinoma), A549 (non-small cell lung cancer) and SW480 (colon carcinoma), as well as in vivo in a Hep3B SCID mouse xeno-transplantation model. 2H-Indazole tautomer stabilization in 1 has been confirmed by X-ray diffraction.

  8. Effect of light on 2H/1H fractionation in lipids from continuous cultures of the diatom Thalassiosira pseudonana

    Science.gov (United States)

    Sachs, Julian P.; Maloney, Ashley E.; Gregersen, Joshua

    2017-07-01

    Continuous cultures of the marine diatom Thalassiosira pseudonana were grown at irradiances between 6 and 47 μmol m-2 s-1 in order to evaluate the effect of light on hydrogen isotope fractionation in lipids. δ2H values increased with irradiance in phytol by 1.1‰ (μmol m-2 s-1)-1 and by 0.3‰ (μmol m-2 s-1)-1 in the C14:0 fatty acid, but decreased by 0.8‰ (μmol m-2 s-1)-1 in the sterol 24-methyl-cholesta-5,24(28)-dien-3β-ol (C28Δ5,24(28)). The anticorrelation between δ2H values in C28Δ5,24(28) and irradiance is attributed to enhanced sterol precursor synthesis via the plastidic methylerythritol phosphate (MEP) pathway at high irradiance, relative to the cytosolic mevalonic acid (MVA) pathway, and the supposition that MEP precursors are 2H-depleted compared to MVA precursors because they incorporate a greater proportion of hydrogen from photosynthetically produced NADPH. Increasing δ2H values of phytol and C14:0 with irradiance is attributed to a greater proportion of pyruvate, the last common precursor to both lipids, being sourced from glycolysis in the mitochondria and cytosol, where enhanced incorporation of metabolic NADPH and further hydrogen exchange with cell water can enrich pyruvate with 2H relative to pyruvate from the chloroplast. Irrespective of the biosynthetic mechanisms responsible for the 2H/1H fractionation response to light, the high sensitivity of lipid δ2H values in T. pseudonana continuous cultures would result in -30‰ to +40‰ variations in δ2H over a 40 μmol m-2 s-1 range in sub-saturating irradiance if expressed in the environment, depending on the lipid.

  9. The histone chaperone Vps75 forms multiple oligomeric assemblies capable of mediating exchange between histone H3-H4 tetramers and Asf1-H3-H4 complexes

    DEFF Research Database (Denmark)

    Hammond, Colin M; Sundaramoorthy, Ramasubramanian; Larance, Mark

    2016-01-01

    Vps75 is a histone chaperone that has been historically characterized as homodimer by X-ray crystallography. In this study, we present a crystal structure containing two related tetrameric forms of Vps75 within the crystal lattice. We show Vps75 associates with histones in multiple oligomers...... catalysed histone H3 K9 acetylation. In the absence of Asf1 this model can be used to generate a complex consisting of a reconfigured Vps75 tetramer bound to a H3-H4 tetramer. This provides a structural explanation for many of the complexes detected biochemically and illustrates the ability of Vps75....... In the presence of equimolar H3-H4 and Vps75, the major species is a reconfigured Vps75 tetramer bound to a histone H3-H4 tetramer. However, in the presence of excess histones, a Vps75 dimer bound to a histone H3-H4 tetramer predominates. We show the Vps75-H3-H4 interaction is compatible with the histone...

  10. Measurements of intracellular volumes by 59Co and 2H/1H NMR and their physiological applications.

    Science.gov (United States)

    Askenasy, Nadir; Navon, Gil

    2005-04-01

    Determination of the intracellular water volumes using NMR spectroscopy was performed using the NMR-visible nuclei: 59Co and 2H or 1H. Accurate measurement of intracellular water in cell suspensions and perfused organs is an important physiological parameter in the context of electrolyte homeostasis and energy metabolism, in particular when these parameters are monitored by non-invasive NMR spectroscopy. Furthermore, repeated or continuous monitoring of intracellular water provided significant insights into the physiology of cardiac muscle and sarcolemmal membrane permeability and integrity.

  11. New modification of the Perkow reaction: halocarboxylate anions as leaving groups in 3-acyloxyquinoline-2,4(1H,3H)-dione compounds

    Science.gov (United States)

    Paleta, Oldřich; Pomeisl, Karel; Kafka, Stanislav; Klásek, Antonín; Kubelka, Vladislav

    2005-01-01

    Substituted 3-(fluoroacyloxy)quinoline-2,4(1H,3H)-diones including 3-(fluoroiodoacetoxy) derivatives react with triethyl phosphite to afford either the product of the Perkow reaction or the corresponding 4-ethoxyquinolin-2(1H)-one. In both reactions, the fluorocarboxylate anion acts as the first observed leaving group. This observation restricts the application of the intramolecular Horner-Wadsworth-Emmons synthesis to modify quinoline-2,4(1H,3H)-diones by the annulation of fluorinated but-2-enolide rings. PMID:16551375

  12. New modification of the Perkow reaction: halocarboxylate anions as leaving groups in 3-acyloxyquinoline-2,4(1H,3H-dione compounds

    Directory of Open Access Journals (Sweden)

    Klásek Antonín

    2005-12-01

    Full Text Available Abstract Substituted 3-(fluoroacyloxyquinoline-2,4(1H,3H-diones including 3-(fluoroiodoacetoxy derivatives react with triethyl phosphite to afford either the product of the Perkow reaction or the corresponding 4-ethoxyquinolin-2(1H-one. In both reactions, the fluorocarboxylate anion acts as the first observed leaving group. This observation restricts the application of the intramolecular Horner-Wadsworth-Emmons synthesis to modify quinoline-2,4(1H,3H-diones by the annulation of fluorinated but-2-enolide rings.

  13. Fabrication of Indocyanine Green and 2H, 3H-perfluoropentane loaded microbubbles for fluorescence and ultrasound imaging

    Science.gov (United States)

    He, Yutong; Wu, Qiang; Ma, Rong; Chang, Shufang; Shao, Pengfei; Xu, Ronald

    2016-03-01

    As a near-infrared (NIR) fluorescence dye, Indocyanine Green (ICG) has not gained broader clinical applications, owing to its multiple limitations such as concentration-dependent aggregation, low fluorescence quantum yield, poor physicochemical stability and rapid elimination from the body. In the meanwhile, 2H,3H-perfluoropentane (H-PFP) has been widely studied in ultrasound imaging as a vehicle for targeted delivery of contrast agents and drugs. We synthesized a novel dual-modal fluorescence and ultrasound contrast agent by encapsulating ICG and H-PFP in lipid microbubbles using a liquid-driven coaxial flow focusing (LDCFF) process. Uniform microbubbles with the sizes ranging from 1-10um and great ICG loading efficiency was achieved by this method. Our benchtop experiments showed that ICG/H-PFP microbubbles exhibited less aggregation, increased fluorescence intensity and more stable photostability compared to free ICG aqueous solution. Our phantom experiments demonstrated that ICG/H-PFP microbubbles enhanced the imaging contrasts in fluorescence imaging and ultrasonography. Our animal experiments indicated that ICG/H-PFP microbubbles extended the ICG life time and facilitated dual mode fluorescence and ultrasound imaging in vivo.

  14. 1-Methyl-3-(2-oxo-2H-chromen-3-yl-1H-imidazol-3-ium picrate

    Directory of Open Access Journals (Sweden)

    Nguyen Van Tuyen

    2013-06-01

    Full Text Available The title salt, C13H11N2O2+·C6H2N3O7−, is the unexpected product of a domino reaction of 3-cyanomethyl-1-methylimidazolium chloride with salicylic aldehyde in the presence of picric acid. In the cation, the 1H-imidazole ring is twisted by 63.2 (1° from the 2H-chromen plane. In the crystal, cations and anions are alternately stacked along the a axis through π–π stacking interactions between the almost parallel aromatic rings [centroid–centroid distances = 3.458 (2 and 3.678 (2 Å]. The stacks are further linked by C—H...O hydrogen bonds into a two-tier layer parallel to (001.

  15. Derivatives of 1,3-disubstituted 2,4(1H,3H)-quinazolinediones as possible peripheral vasodilators or antihypertensive agents.

    Science.gov (United States)

    Havera, H J; Vidrio, H

    1979-12-01

    A series of 1,3-disubstituted 2,4(1H,3H)-quinazolinediones was prepared from the 3-substituted 2,4(1H,3H)-quinazolinediones by treatment with sodium hydride and the desired alkyl halide in xylene. These compounds showed varying degrees of vasodilation and antihypertensive activity without significant blockade of alpha-adrenergic receptors. 1-[3-(N,N-Dimethylamino)propyl]-3-[3-(4-phenyl1-piperazinyl)propyl]-2,4(1H,3H)-quinazolinedione, which was selected for further studies, was more potent than papaverine in inducing vasodilation and induced a prolonged decrease in systolic blood pressure of hypertensive rats upon oral administration.

  16. Nqrs Data for C3H10INO6 [C3H7NO2·HIO3·(1/2)(H2O)] (Subst. No. 0642)

    Science.gov (United States)

    Chihara, H.; Nakamura, N.

    This document is part of Subvolume A `Substances Containing Ag … C10H15' of Volume 48 `Nuclear Quadrupole Resonance Spectroscopy Data' of Landolt-Börnstein - Group III `Condensed Matter'. It contains an extract of Section `3.2 Data tables' of the Chapter `3 Nuclear quadrupole resonance data' providing the NQRS data for C3H10INO6 [C3H7NO2·HIO3·(1/2)(H2O)] (Subst. No. 0642)

  17. Water - Isotope - Map (δ 18O, δ 2H, 3H) of Austria: Applications, Extremes and Trends

    Science.gov (United States)

    Wyhlidal, Stefan; Kralik, Martin; Benischke, Ralf; Leis, Albrecht; Philippitsch, Rudolf

    2016-04-01

    The isotopic ratios of oxygen and hydrogen in water (2H/1H and 18O/16O) are important tools to characterise waters and their cycles. This starts in the atmosphere as rain or snow and continues in surface water and ends in shallow groundwater as well as in deep groundwater. Tritium formed by natural cosmic radiation in the upper atmosphere and in the last century by tests of thermonuclear bombs in the atmosphere, is characterised by its radioactive decay with a half-life of 12.32 years and is an ideal age-marker during the last 60 years. To determine the origin and mean age of waters in many projects concerning water supply, engineering and scientific projects in the last 45 years on more than 1,350 sites, more than 40,000 isotope measurements were performed in Austria. The median value of all sites of oxygen-18 is δ 18O -10.7 ‰ and for hydrogen-2 δ 2H -75 ‰. As the fractionation is mainly temperature dependent the lowest negative values are observed in winter precipitation (oxygen-18 as low as δ 18O -23 ‰) and in springs in the mountain regions (δ 18O -15.1 ‰). In contrast the highest values were observed in summer precipitation (up to δ 18O - 0.5 ‰) and in shallow lakes in the Seewinkel (up to δ 18O + 5 ‰). The isotopic ratios of the Austrian waters are also influenced by the origin of the evaporated water masses. Therefore the precipitation in the region south of the main Alpine crest (East-Tyrol, Carinthia and South-East Styria) is approximately 1 ‰ higher in δ 18O-values than sites at the same altitude in the northern part. This is most probably caused by the stronger influence of precipitation from the mediterranean area. The median value of all 1,120 sampling sites of decay corrected (2015) tritium measurements is 6.2 tritium units (TU). This is somewhat smaller than the median value of all precipitation stations with 7.2 TU. This can be explained by the fact that in most cases in groundwater the median value has been reduced by decay

  18. Copper-catalyzed C(sp(3))-H functionalization of ketones with vinyl azides: synthesis of substituted-1H-pyrroles.

    Science.gov (United States)

    Donthiri, Ramachandra Reddy; Samanta, Supravat; Adimurthy, Subbarayappa

    2015-10-28

    Copper-catalyzed C(sp(3))-H functionalization of ketones with vinyl azides for the synthesis of substituted pyrroles has been developed. The method is a straightforward and efficient way to access a series of 2,3,5-trisubstituted-1H-pyrroles in modest to excellent yields with broad functional group tolerance under mild conditions.

  19. A facile and convenient approach for the one-pot synthesis of 2,4(1H,3H)-quinazolinediones

    Institute of Scientific and Technical Information of China (English)

    Mahnaz Sharafi-Kolkeshvandi; Farzad Nikpour

    2012-01-01

    A fast and efficient method is described for the one-pot synthesis of 2,4(1H,3H)-quinazolinediones by cyclization reaction of anthranilic acid derivatives with potassium cyanate and acetic acid in PEG.Good to high yields of the products obtain in short reaction times with simple work-up.

  20. Effect of salinity on 2H/1H fractionation in lipids from continuous cultures of the coccolithophorid Emiliania huxleyi

    Science.gov (United States)

    Sachs, Julian P.; Maloney, Ashley E.; Gregersen, Josh; Paschall, Christopher

    2016-09-01

    Salinity and temperature dictate the buoyancy of seawater, and by extension, ocean circulation and heat transport. Yet there remain few widely applicable proxies for salinity with the precision necessary to infer all but the largest hydrographic variations in the past. In the last decade the hydrogen isotope composition (2H/1H or δ2H) of microalgal lipids has been shown to increase systematically with salinity, providing a foundation for its use as a paleosalinity proxy. Culture and field studies have indicated a wide range of sensitivities for this response, ranging from about 0.6-3.3‰ ppt-1 depending on the lipid, location and/or culturing conditions. Lacking in these studies has been the controlled conditions necessary to isolate the response to salinity while keeping all other growth parameters constant. Here we show that the hydrogen isotope composition of lipids in the marine coccolithophorid Emiliania huxleyi grown in chemostats increased by 1.6 ± 0.3‰ ppt-1 (p < 0.05) in eight individual alkenones and by 2.0 ± 0.1‰ ppt-1 (p < 0.05) in three individual fatty acids over the salinity range 20-42 ppt. Hydrogen isotope ratios of phytol and the sterol 24-methyl-cholest-5,22-dien-3β-ol (brassicasterol) also increased with salinity but correlations were weaker than for the acetogenic lipids. For eight individual alkenones, linear regression analyses of the fractionation factors on salinity yielded slopes of 1.2-2.2‰ ppt-1. This sensitivity of δ2Halkenone to salinity is 45-71% of that previously reported for E. huxleyi, which can be attributed to the fact that previous experiments were performed with batch cultures in which growth rates and other parameters differed between salinity treatments. The underlying cause of this response to salinity remains unknown, but may result from changes in (1) the proportion of lipid hydrogen derived from NADPH versus water, (2) the proportion of lipid hydrogen derived from NADPH from Photosystem I versus the oxidative

  1. New pyrazole derivative 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole: synthesis and assessment of some biological activities.

    Science.gov (United States)

    de Oliveira, Lanussy Porfiro; da Silva, Daiany Priscilla Bueno; Florentino, Iziara Ferreira; Fajemiroye, James Oluwagbamigbe; de Oliveira, Thiago Sardinha; Marcelino, Renato Ivan de Ávila; Pazini, Francine; Lião, Luciano Morais; Ghedini, Paulo César; de Moura, Soraia Santana; Valadares, Marize Campos; de Carvalho, Verônica Vale; Vaz, Boniek Gontijo; Menegatti, Ricardo; Costa, Elson Alves

    2017-01-01

    The molecular modification and synthesis of compounds is vital to discovering drugs with desirable pharmacological and toxicity profiles. In response to pyrazole compounds' antipyretic, analgesic, and anti-inflammatory effects, this study sought to evaluate the analgesic, anti-inflammatory, and vasorelaxant effects, as well as the mechanisms of action, of a new pyrazole derivative, 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole. During the acetic acid-induced abdominal writhing test, treatments with 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole reduced abdominal writhing, while during the formalin test, 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole reduced licking times in response to both neurogenic pain and inflammatory pain, all without demonstrating any antinociceptive effects, as revealed during the tail flick test. 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole also reduced carrageenan-induced paw edema and cell migration during the carrageenan-induced pleurisy test. As demonstrated by the model of the isolated organ, 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole exhibits a vasorelaxant effect attenuated by Nω-nitro-l-arginine methyl ester, 1H-[1,2,4]oxadiazolo[4,3-alpha]quinoxalin-1-one, tetraethylammonium or glibenclamide. 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole also blocked CaCl2 -induced contraction in a dose-dependent manner. Suggesting a safe toxicity profile, 5-[1-(4-fluorophenyl)-1H-pyrazol-4-yl]-2H-tetrazole reduced the viability of 3T3 cells at higher concentrations and was orally tolerated, despite signs of toxicity in doses of 2000 mg/kg. Lastly, the compounds' analgesic activity might be attributed to the involvement of the NO/cGMP pathway and K(+) channels observed in the vasorelaxant effect.

  2. Heats of formation and thermodynamic functions for C2H, C3H, and C4H from 300 K to 6000 K

    Science.gov (United States)

    Saturno, A. F.

    1982-01-01

    A review of the energy level and heat of formation data for the species C2H, C3H, and C4H is given. The procedure for computing thermochemical data from partition function is also reviewed. Working expressions for approximate partition functions, free-energy function, enthalpy function, and heat capacity for a linear polyatomic species are presented.

  3. Updated evidences of the Trojan Horse particle invariance for $^2$H(d,p)$^3$H reaction

    CERN Document Server

    Pizzone, R G; Bertulani, C A; Mukhamedzhanov, A M; Blokhintsev, L; La Cognata, M; Lamia, L; Rinollo, A; Spartá, R; Tumino, A

    2012-01-01

    The Trojan Horse nucleus invariance for the binary d(d,p)t reaction was tested using the quasi free $^2$H($^6$Li, pt)$^4$He and $^2$H($^3$He,pt)H reactions after $^6$Li and $^3$He break-up, respectively. The astrophysical S(E)-factor for the d(d,p)t binary process was then extracted in the framework of the Plane Wave Approximation applied to the two different break-up schemes. The obtained results are compared with direct data as well as with previous indirect investigations. The very good agreement confirms the applicability of the Plane Wave Approximation and suggests the independence of binary indirect cross section on the chosen Trojan Horse nucleus also for the present case.

  4. A general and efficient approach to 2H-indazoles and 1H-pyrazoles through copper-catalyzed intramolecular N-N bond formation under mild conditions.

    Science.gov (United States)

    Hu, Jiantao; Cheng, Yongfeng; Yang, Yiqing; Rao, Yu

    2011-09-28

    A new efficient copper-catalyzed intramolecular amination reaction has been developed to readily synthesise a wide variety of multi-substituted 2H-indazole and 1H-pyrazole derivatives from easily accessible starting materials under mild conditions. A highly selective ligand for estrogen receptor β was prepared in three steps by employing this method.

  5. Synthesis and biological evaluation of novel 2,4,5-triaryl-1 H-pyrazol-3(2H)-ones as inhibitors of ALK5

    Institute of Scientific and Technical Information of China (English)

    Xing Zhou Li; Xian Ping Dai; Kang Ying Lai; Li Li Wang; Zhi Bing Zheng; Song Li

    2008-01-01

    A series of 2,4,5-triaryl substituted 1H-pyrazol-3(2H)-ones,as ALK5 inhibitors,were desigened,synthesized and evaluated in vitro.Most compounds exhibited noticeable ALK5 inhibition activities at 1 μmol/L and displayed no significant cytotoxicities at 30 μmol/L.

  6. Iodido[5-methyl-1H-benzimidazole-2(3H-thione-κS]bis(triphenylphosphane-κPcopper(I methanol monosolvate

    Directory of Open Access Journals (Sweden)

    Yu-Han Jiang

    2012-10-01

    Full Text Available In the title compound, [CuI(C8H8N2S(C18H15P2]·CH3OH, the coordination environment around the CuI atom is distorted tetrahedral, defined by two P atoms of two triphenylphosphane ligands, one S atom of a 5-methyl-1H-benzimidazole-2(3H-thione ligand and one I atom. The complex molecules and the methanol solvent molecules are connected via N—H...O and O—H...I hydrogen bonds, forming a chain along [010]. An intramolecular N—H...I hydrogen bond is also observed.

  7. Synthesis and Antitumor Evaluation of Novel 5-Hydrosulfonyl-1H-benzo[d]imidazol-2(3H-one Derivatives

    Directory of Open Access Journals (Sweden)

    Guang Ouyang

    2016-04-01

    Full Text Available A series of novel 5-hydrosulfonyl-1H-benzo[d]imidazol-2(3H-one derivatives bearing natural product substructures has been successfully synthesized and their antitumor activity studied. These newly synthesized derivatives were characterized by 1H-NMR, 13C-NMR and high resolution mass spectral data, then screened as antitumor agents against the A549, HCC1937, and MDA-MB-468 human tumor cell lines using MTT cell proliferation assays. The results show that some of these compounds can effectively inhibit the growth of these cancerous cells, with compound 5b being the best one (IC50 = 2.6 μM. Flow cytometry data revealed that compound 5b induced apoptosis of HCC1937 cells with increased solution concentration. The structure and activity relationships (SAR of these compounds is summarized.

  8. The distribution of radioactive ( 3H, 14C) and stable ( 2H, 18O) isotopes in precipitation, surface and groundwaters of NW Yugoslavia

    Science.gov (United States)

    Horvatinčić, Nada; Krajcar-Bronić, Ines; Pezdič, Jože; Srdoč, Dušan; Obelić, Bogomil

    1986-11-01

    The isotopic measurements ( 2H, 3H, 18O) of precipitiation in Zagreb (since 1976) and Ljubljana (since 1981) in NW Yugoslavia show seasonal variations typical of the Northern hemisphere. Continuous measurements of tritium concentration in the Sava River ca 10 km upstream from Zagreb have been performed since 1976. Data show a smooth line without periodical changes, but a steady decrease is obvious. The sampling place is situated ca 30 km downstream from the Kr\\vsko Nuclear Power Plant. No change in tritium concentration due to the operation of the power plant has been observed. A comprehensive program of monitoring of the 14C activity in air CO 2 as well as in vegetables, cereals and tree-rings in the surroundings of the Nuclear Power Plant Kr\\vsko has been carried out since 1984. The measurement of 2H and 18O in karst springs of the Korana River catchmet area (Plitvice National Park) gave a meteoric water line equal to δ2H = 7.9 δ18O + 8.5, which is typical of the NW part of Yugoslavia. A fairly constant concentration of 2H and 18O in spring water indicates a thorough mixing of water in the karst aquifers. The mean residence time (MRT) of karst water was determined by measuring monthly tritium activity of spring water. The MRT is very short, ranging between 1 and 4 years on average.

  9. Search for protons from the 2H(d,p)3H reaction in an electrolytic cell with Pd-Pt electrodes

    Science.gov (United States)

    Rehm, K. E.; Kutschera, W.; Perlow, G. J.

    1990-01-01

    The production of protons from the 2H(d,p)3H reaction was investigated using an electrolytic cell and a proportional counter. The cathode, consisting of a 30.5-mg/cm2-thick Pd foil, separated the gas in the counter from the electrolyte (0.1M LiOD in D2O). The efficiency for proton detection was 28%. The electrolytic cell was operated with current densities up to 650 mA/cm2. Several runs with the current switched on and off and with different Pd foils have been performed with the longest run lasting more than 10 days. No difference in the count rate was observed when the electrolytic cell was on or off. From the high-energy part of the particle spectrum we obtain an upper limit for the proton production from the fusion reaction 2H(d,p)3H of 4×10-23 fusion/(dd pair/sec).

  10. sup 4 He sup 1 H sub 2 sup + and sup 4 He sup 2 H sup + , exotic impurities in sup 6 He sup + beam

    CERN Document Server

    Miljanic, D; Aliotta, M; Cherubini, S; Davinson, T; Di Pietro, A; Figuera, P; Gaelens, M; Galster, W; Loiselet, M; Ninane, A; Ostrowski, A N; Ryckewaert, G; Shotter, A C; Soic, N; Spitaleri, C

    2000-01-01

    sup 4 He sup 1 H sub 2 sup + ions were observed as an impurity in a 17.0 MeV sup 6 He sup + beam produced by CYCLONE, with the ratio of intensities being 1 : 5400. A sup 4 He sup 2 H sup + beam was also observed, having 60 times weaker intensity and slightly lower magnetic rigidity than original sup 6 He sup + beam.

  11. (2) H/(1) H measurements of amphiboles and nominally anhydrous minerals (clinopyroxene, garnetand diamond)usinghigh-temperatureCF-EA-PY-IRMS.

    Science.gov (United States)

    Fourel, François; Lécuyer, Christophe; Demeny, Attila; Boulvais, Philippe; Lange, Lutz; Jacob, Dorrit E; Kovacs, Istvan

    2017-09-20

    We have used ahigh-precision, high efficiency method for themeasurementof the(2) H/(1) H ratios of hydrous silicates (amphiboles) and nominally anhydrous minerals (NAM) such as clinopyroxene, garnet and diamond, which are usually extremely resistant to pyrolysis. This opens up new fields of investigation to better understand the conditionsof formation fordeep-Earth minerals. The technique described hereinvolvesIsotopic Ratio Mass Spectrometry (IRMS) online in continuous flow mode with an Elemental Analyzer (EA) using"purge and trap" technology rather than conventional packed column-GC gas separation. The system is equipped with a special high temperature furnace reaching 1500°C, with a longer hot zone and improved temperature stability. Emphasis is put on the efficiency of the system to reliably pyrolyserefractory minerals difficult to analyse with other conventional systems. While conventional systems usually fail to generate hydrogen suitable for isotopic analyses, with the technique presented here we were able to measure (2) H/(1) H ratios from 4diamond samples (δ(2) H= -60, -77, -84 and -79‰ V-SMOW; average SD =4.5‰; n=2),3 garnet samples (δ(2) Hfrom -70 to -63‰), and 9 clinopyroxenes (δ(2) H from -92 to -58‰) associated with7 amphiboles (δ(2) Hfrom -76 to -27‰) from single mantle rock. The possibility of using such a system to reliably measure (2) H/(1) H ratios from refractory minerals, which are usually extremely difficult to analyse, offers a new tool of investigation for giving us unrivaled clues to study the Earth's deep interiors. This article is protected by copyright. All rights reserved.

  12. Synthesis and Antitumor Evaluation of Novel 5-Hydrosulfonyl-1H-benzo[d]imidazol-2(3H)-one Derivatives.

    Science.gov (United States)

    Ouyang, Guang; Tong, Rongsheng; Li, Jinqi; Bai, Lan; Ouyang, Liang; Duan, Xingmei; Li, Fengqiong; He, Pin; Shi, Jianyou; He, Yuxin

    2016-04-20

    A series of novel 5-hydrosulfonyl-1H-benzo[d]imidazol-2(3H)-one derivatives bearing natural product substructures has been successfully synthesized and their antitumor activity studied. These newly synthesized derivatives were characterized by ¹H-NMR, (13)C-NMR and high resolution mass spectral data, then screened as antitumor agents against the A549, HCC1937, and MDA-MB-468 human tumor cell lines using MTT cell proliferation assays. The results show that some of these compounds can effectively inhibit the growth of these cancerous cells, with compound 5b being the best one (IC50 = 2.6 μM). Flow cytometry data revealed that compound 5b induced apoptosis of HCC1937 cells with increased solution concentration. The structure and activity relationships (SAR) of these compounds is summarized.

  13. Synthesis and SAR of 1-Hydroxy-1H-benzo[d]imidazol-2(3H)-ones as Inhibitors of d-Amino Acid Oxidase

    Science.gov (United States)

    2012-01-01

    A series of 1-hydroxy-1H-benzo[d]imidazol-2(3H)-ones were synthesized and evaluated for their ability to inhibit human and porcine forms of d-amino acid oxidase (DAAO). The inhibitory potency is largely dependent on the size and position of substituents on the benzene ring with IC50 values of the compounds ranging from 70 nM to greater than 100 μM. Structure–activity relationships of this new class of DAAO inhibitors will be presented in detail along with comparisons to previously published SAR data from other classes of DAAO inhibitors. Two of these compounds were given to mice orally together with d-serine to assess their effects on plasma d-serine pharmacokinetics. PMID:23243487

  14. 5-[(3-Fluorophenyl(2-hydroxy-6-oxocyclohex-1-en-1-ylmethyl]-6-hydroxy-1,3-dimethylpyrimidine-2,4(1H,3H-dione

    Directory of Open Access Journals (Sweden)

    Assem Barakat

    2016-09-01

    Full Text Available 5-[(3-Fluorophenyl(2-hydroxy-6-oxocyclohex-1-en-1-yl-methyl]-6-hydroxy-1,3-di-methylpyrimidine-2,4(1H,3H-dione 3 was synthesized via a multicomponent reaction. The Aldol–Michael addition reactions of N,N-dimethylbarbituric acid, cyclohexane-1,3-dione, and 3-fluorobenzaldehyde in aqueous solution gave the product in high yield. The molecular structure of the compound was confirmed by spectroscopic methods and X-ray crystallography. The title compound (C19H19FN2O5·H2O crystallizes in the Monoclinic form, P21/c, a = 7.8630 (5 Å, b = 20.0308 (13 Å, c = 11.3987 (8 Å, β = 104.274 (3°, V = 1739.9 (2° Å3, Z = 4, Rint = 0.117, wR(F2 = 0.124, T = 100 K.

  15. Synthesis and Crystal Structure of 1-(4-Nitrobenzyl-3-allyl-1H-benzo[d]imidazol-2(3H-one

    Directory of Open Access Journals (Sweden)

    Dounia Belaziz

    2013-01-01

    Full Text Available A functionalized benzimidazole, 1-(4-nitrobenzyl-3-allyl-1H-benzo[d]imidazol-2(3H-one, has been synthesized, and the crystal structure was determined and analyzed. This compound crystallizes in the monoclinic, space group P21/n (number 14 c with cell parameters, a=7.12148(8 Å, b=16.12035(17 Å, c=13.04169(17 Å, β=93.3043(11, V=1494.71(3 Å3, and Dcalc = 1.375 g/mm3. The solid state geometry is stabilized by intermolecular π–π interactions along with the van der Waals interactions which contribute to the stability of the crystal packing. Computational calculations have been used to properly understand the main intermolecular interactions present in the crystal.

  16. Synthesis of Z- and E-[2,3-{sup 2}H{sub 2}] and [2,3-{sup 3}H{sub 2}]-1,1-dichloro-2,3-diphenylcyclopropane ({sup 2}H-and {sup 3}H-analog II and its trans isomer)

    Energy Technology Data Exchange (ETDEWEB)

    Day, B.W.; Jonnalagadda, S.S. [Pittsburgh Univ., PA (United States). Dept. of Occupational Health

    1995-01-01

    {sup 2}H and {sup 3}H labeled Z- and E-1,1-dichloro-2,3-diphenylcyclopropane (1 and 2) were synthesized starting from NaB{sup 2}H{sub 4} and NaB{sup 3}H{sub 4} reduction of benzil. The resulting glycols were transformed to the 1,2-labeled Z- and E-stilbenes by thermolysis of their cyclic thionocarbonates in trimethylphosphite. The stilbenes were reacted with phase transfer-generated dichlorocarbene to form the title compounds. The dideuterio isomers were separated by fractional crystallization in yields of 60 and 48%. Each was greater than 99% geometrically and 98% isotopically pure. The ditritio isomers were separated by C-18 HPLC. The radiochemical yields, on a molar basis using benzil as the limiting reagent, were 42% and 23%, each with specific activity of 88.5 mCi/mmol and radiochemical purity of >95%. (Author).

  17. Hysteresis effect of ammonium and water protons by 1H MAS NMR in (NH4)2CuBr4·2H2O

    Science.gov (United States)

    Lim, Ae Ran; Cho, Jiung

    2017-10-01

    The chemical shifts, linewidths, and spin-lattice relaxation times for ammonium and water protons in (NH4)2CuBr4·2H2O were investigated by 1H magic angle spinning nuclear magnetic resonance (MAS NMR) with a focus on the roles of NH4+ and H2O at high temperatures. The changes in the temperature dependence of the data near Td (=360 K) were related to variations of the H environments; the mechanism above Td was related to hydrogen-bond transfer involving breakage of the weak part of the hydrogen bond. The hysteresis effects for the ammonium and water protons in (NH4)2CuBr4·2H2O by MAS NMR were described with respect to heating and cooling.

  18. The Davis-Beirut reaction: N1,N2-disubstituted-1H-indazolones via 1,6-electrophilic addition to 3-alkoxy-2H-indazoles.

    Science.gov (United States)

    Conrad, Wayne E; Fukazawa, Ryo; Haddadin, Makhluf J; Kurth, Mark J

    2011-06-17

    A variety of electrophiles (anhydrides, acid chlorides, carbonochloridates, sulfonyl chlorides, and alkyl bromides) react with 3-methoxy-2H-indazole (1a), benzoxazin[3,2-b]indazole (1d), and oxazolino[3,2-b]indazole (1e) - substrates available by the Davis-Beirut reaction - to yield a diverse set of N(1),N(2)-disubstituted-1H-indazolones. With certain electrophiles, an AERORC (Addition of the Electrophile, Ring Opening, and Ring Closure) process on indazole 1d results in indazoloindazolone formation. An intriguing aspect of these N(1),N(2)-disubstituted-1H-indazolones is that they are poised for diversification through, for example, azide-alkyne cycloaddition chemistry reported here.

  19. Chlorido[5-methoxy-1H-benzimidazole-2(3H-thione-κS]bis(triphenylphosphane-κPcopper(I methanol disolvate

    Directory of Open Access Journals (Sweden)

    Qing-Xuan Meng

    2014-02-01

    Full Text Available In the title complex, [CuCl(C8H8N2OS(C18H15P2]·2CH3OH, the CuI ion is coordinated by one chloride anion, one S atom from the 5-methoxy-1H-benzimidazole-2(3H-thione ligand and two P atoms from two triphenylphosphine ligands in a distorted tetrahedral geometry. One of the N-bound H atoms is involved in an intramolecular N—H...Cl hydrogen bond, while another one interacts with the solvent methanol molecule via an N—H...O hydrogen bond. Intermolecular O—H...Cl and O—H...O hydrogen bonds link two further complex molecules and four solvent molecules into a centrosymmetric structural unit. The short distance of 3.624 (4 Å between the centroids of the five- and the six-membered rings of two benzimidazole fragments indicates the presence of π–π interactions.

  20. Study of the A(e,e'$\\pi^+$) Reaction on $^1$H, $^2$H, $^{12}$C, $^{27}$Al, $^{63}$Cu and $^{197}$Au

    Energy Technology Data Exchange (ETDEWEB)

    Qian, X; Clasie, B; Arrington, J; Asaturyan, R; Benmokhtar, F; Boeglin, W; Bosted, P; Bruell, A; Christy, M E; Chudakov, E; Dalton, M M; Daniel, A; Day, D; Dutta, D; El Fassi, L; Ent, R; Fenker, H C; Ferrer, J; Fomin, N; Gao, H; Garrow, K; Gaskell, D; Gray, C; Huber, G M; Jones, M K; Kalantarians, N; Keppel, C E; Kramer, K; Li, Y; Liang, Y; Lung, A F; Malace, S; Markowitz, P; Matsumura, A; Meekins, D G; Mertens, T; Miyoshi, T; Mkrtchyan, H; Monson, R; Navasardyan, T; Niculescu, G; Niculescu, I; Okayasu, Y; Opper, A K; Perdrisat, C; Punjabi, V; Rauf, A W; Rodriquez, V M; Rohe, D; Seely, J; Segbefia, E; Smith, G R; Sumihama, M; Tadevosyan, V; Tang, L; Villano, A; Vulcan, W F; Wesselmann, F R; Wood, S A; Yuan, L; Zheng, X

    2010-05-01

    Cross sections for the p($e,e'\\pi^{+}$)n process on $^1$H, $^2$H, $^{12}$C, $^{27}$Al, $^{63}$Cu and $^{197}$Au targets were measured at the Thomas Jefferson National Accelerator Facility (Jefferson Lab) in order to extract the nuclear transparencies. Data were taken for four-momentum transfers ranging from $Q^2$=1.1 to 4.8 GeV$^2$ for a fixed center of mass energy of $W$=2.14 GeV. The ratio of $\\sigma_L$ and $\\sigma_T$ was extracted from the measured cross sections for $^1$H, $^2$H, $^{12}$C and $^{63}$Cu targets at $Q^2$ = 2.15 and 4.0 GeV$^2$ allowing for additional studies of the reaction mechanism. The experimental setup and the analysis of the data are described in detail including systematic studies needed to obtain the results. The results for the nuclear transparency and the differential cross sections as a function of the pion momentum at the different values of $Q^2$ are presented. Global features of the data are discussed and the data are compared with the results of model calculations for the p($e,e'\\pi^{+}$)n reaction from nuclear targets.

  1. Integration of the barley genetic and seed proteome maps for chromosome 1H, 2H, 3H, 5H and 7H

    DEFF Research Database (Denmark)

    Finnie, Christine; Bagge, Merethe; Steenholdt, Torben;

    2009-01-01

    between cultivar traits, proteome and genome. Proteome analysis of doubled haploid lines derived from a cross between a malting (Scarlett) and a feed cultivar (Meltan) enabled genetic localisation of protein phenotypes represented by 48 spot variations, involving e.g. peroxidases, serpins, alpha-amylase/trypsin...... inhibitors, peroxiredoxin and a small heat shock protein, in relation to markers on the chromosome map....

  2. Integration of the barley genetic and seed proteome maps for chromosome 1H, 2H, 3H, 5H and 7H.

    Science.gov (United States)

    Finnie, Christine; Bagge, Merethe; Steenholdt, Torben; Østergaard, Ole; Bak-Jensen, Kristian Sass; Backes, Gunter; Jensen, Anaïs; Giese, Henriette; Larsen, Jørgen; Roepstorff, Peter; Svensson, Birte

    2009-02-01

    Two-dimensional gel electrophoresis was used to screen spring barley cultivars for differences in seed protein profiles. In parallel, 72 microsatellite (simple sequence repeat (SSR)) markers and 11 malting quality parameters were analysed for each cultivar. Over 60 protein spots displayed cultivar variation, including peroxidases, serpins and proteins with unknown functions. Cultivars were clustered based on the spot variation matrix. Cultivars with superior malting quality grouped together, indicating malting quality to be more closely correlated with seed proteomes than with SSR profiles. Mass spectrometry showed that some spot variations were caused by amino acid differences encoded by single nucleotide polymorphisms (SNPs). Coding SNPs were validated by mass spectrometry, expressed sequence tag and 2D gel data. Coding SNPs can alter function of affected proteins and may thus represent a link between cultivar traits, proteome and genome. Proteome analysis of doubled haploid lines derived from a cross between a malting (Scarlett) and a feed cultivar (Meltan) enabled genetic localisation of protein phenotypes represented by 48 spot variations, involving e.g. peroxidases, serpins, alpha-amylase/trypsin inhibitors, peroxiredoxin and a small heat shock protein, in relation to markers on the chromosome map.

  3. Asymmetry in the N-inversion of heteroarene imines: pyrimidin-4(3H)-imine, pyridin-2(1H)-imine, and 1H-purine-6(9H)-imine.

    Science.gov (United States)

    Glaser, Rainer; Yin, Jian; Miller, Stephanie

    2010-02-19

    The uncatalyzed, thermal N-inversion reactions were studied of pyrimidin-4(3H)-imine (PMI), pyridin-2(1H)-imine (PYI), and 1H-purine-6(9H)-imine (PUI). Relevant regions of the potential energy surfaces were explored with second-order Moller-Plesset perturbation theory (MP2(full)/6-31G(d)) and with coupled cluster theory (CCSD/6-31G(d), CCSD/6-31+G(d)). The thermochemistry of stationary structures was evaluated at the MP2 level and their energies also were computed at the levels CCSD(T)/6-311+G(d,p) and CCSD(T)/6-311+G(2df,2p) and with structures optimized at lower CCSD levels. The best estimates for the (E)-preference free enthalpies DeltaG(298)(Z vs. E) are 2.6 (PMI), 2.3 (PYI), and 6.0 (PUI) kcal/mol and for the free enthalpies of activation DeltaG(298)(Z --> E) they are 21.6 (PMI), 21.1 (PYI) and 19.7 (PUI) kcal/mol. Nonplanar N-inversion transition state (ITS) structures occur along enantiomeric reaction paths and stationary structures for in-plane N-inversion correspond to second-order saddle points (SOSP) on the potential energy surface. The deformation energy DeltaE(def) = E(SOSP) - E(ITS) is less than 0.5 kcal/mol for PMI and PUI, but it is as high as DeltaE(def) approximately = 2 kcal/mol for PYI. The detailed study of structures and electronic structures along the entire N-inversion path of the isomerization (Z)-PMI (E)-PMI revealed a remarkable stabilization due to asymmetry in the ascent region from the (E)-isomer to ITS. Structures in this region of the potential energy surface allow best for additional bonding overlaps in the HOMO, and this amidine effect predicts lower N-inversion barriers in analogous imines with (Z)-preference energies. The discussion of the halogen-bonded aggregate PMI x ClCH(3) exemplifies that the asymmetry in N-inversion paths is retained and perhaps even enhanced in chlorinated solvents of low polarity.

  4. Synthesis, cytotoxic activity, and tubulin polymerization inhibitory activity of new pyrrol-2(3H)-ones and pyridazin-3(2H)-ones.

    Science.gov (United States)

    Abbas, Samar Hafez; Abuo-Rahma, Gamal El-Din A A; Abdel-Aziz, Mohamed; Aly, Omar M; Beshr, Eman A; Gamal-Eldeen, Amira M

    2016-06-01

    A series of new pyrrol-2(3H)-ones 4a-f and pyridazin-3(2H)-ones 7a-f were synthesized and characterized using different spectroscopic tools. Some of the tested compounds revealed moderate activity against 60 cell lines. The E form of the pyrrolones 4 showed good cytotoxic activity than both the Z form and the corresponding open amide form. Furthermore, the in vitro cytotoxic activity against HepG2 and MCF-7 cell lines revealed that compounds (E)4b, 6f and 7f showed good cytotoxic activity against HepG2 with IC50 values of 11.47, 7.11 and 14.80μM, respectively. Compounds (E)4b, 6f, 7d and 7f showed a pronounced inhibitory effect against cellular localization of tubulin. Flow cytometric analysis indicated that HepG2 cells treated with (E)4b showed a predominated growth arrest at the S-phase compared to that of G2/M-phase. Molecular modeling study using MOE® program indicated that most of the target compounds showed good binding of β-subunit of tubulin with the binding free energy (dG) values about -10kcal/mole.

  5. Synthesis of 1-[6-Fluoro-(2S)-3H,4H-dihydro-2H-2-chromenyl]-(1R)-1,2- ethanediol and 1-[6-Fluoro-(2R)-3H,4H-dihydro-2H-2-chromenyl]- (1R)-1,2-ethanediol

    Institute of Scientific and Technical Information of China (English)

    YU,An-Guang; WANG,Nai-Xing; ZHANG,Jun-Ping; YANG,Yun-Xu; WANG,Wu-Wei; SHENG,Rui-Long

    2004-01-01

    @@ Benzopyran compounds possess diverse pharmacological properties such as β-blockade, anticonvulsant and antimicrobial.[1,2] Our interest has been focused on the synthesis of 1-[6-Fluoro-2S]-3H,4H-dihydro-2H-2-chromenyl]-(1R)-1,2-ethanediol (6) and 1-[6-fluoro-(2R)-3H,4H-dihydro-2H-2-chromenyl]-(1R)-1,2-ethanediol (7) which are particularly convenient precursor to (S,R,R,R)-NE (8). 8 containing four asymmetrical carbon atoms was reported to be the most active isomer.[3] Chandrasekhar[4] has reported on the synthesis of 8. The key step to synthesize this compound is to obtain the chiral chromanone 6 and 7. 6 was accomplished in 8 steps by the Clasien rearrangement and a one-pot Sharpless asymmetric epoxidation, but the compound 7 was accomplished in 10 steps. Johannes[5] used Zr-catalytic kinetic resolution of allylic ethers and Mo-catalyzed chromene formation to synthesize 8 in 14 steps. However both of the methods request many synthetic steps and expensive reagents.

  6. Spin–spin coupling in the HD molecule determined from {sup 1}H and {sup 2}H NMR experiments in the gas-phase

    Energy Technology Data Exchange (ETDEWEB)

    Garbacz, Piotr, E-mail: pgarbacz@chem.uw.edu.pl

    2014-10-31

    Highlights: • The spin–spin coupling constant of the HD molecule is equal to 43.136(7) Hz at 300 K. • Peak-to-peak separations between HD multiplet peaks, J{sub eff}, are smaller than J (D, H). • Nuclear relaxation and intermolecular interactions have an influence on J{sub eff}. • J{sub eff} determined from the {sup 1}H NMR spectrum is smaller than from the {sup 2}H NMR spectrum. - Abstract: The indirect spin–spin coupling of hydrogen deuteride, J(D, H), was determined from a series of {sup 1}H and {sup 2}H NMR spectra acquired at various densities of gaseous solvents (He, Ar, CO{sub 2}, and N{sub 2}O). The analysis of these spectra shows that accurate determination of J(D, H) from this experimental data requires careful examination of the effects of nuclear relaxation and of HD–solvent gas interactions on hydrogen deuteride line shapes. Particularly, it was found that the first-order corrections of the peak-to-peak separations between HD multiplet peaks due to weak van der Waals interactions are proportional to solvent gas density, while these corrections for nuclear relaxation of the proton and the deuteron are proportional to the second power of the inverse of the gas density. Analysis of the data indicates that J(D, H), obtained by correcting for the effects of nuclear relaxation and intermolecular interactions, is 43.136(7) Hz at 300 K.

  7. Synthesis and Structural Studies of Transition Metal Complexes with Bidentate Schiff Base Derived from 3-Acetyl-6-methyl-(2H-pyran-2,4(3H-dione

    Directory of Open Access Journals (Sweden)

    Praveen S. Mane

    2011-01-01

    Full Text Available The solid complexes of Cu(II, Ni(II, Co(II, Mn(II and Fe(III with Schiff base ligands derived from heterocyclic compounds 3-acetyl-6-methyl-(2H-pyran-2,4(3H-dione (Dehydroacetic acid and o-chloroaniline were synthesized and characterized by elemental analysis, conductance, magnetic, thermal, UV-Vis and 1H-NMR spectroscopy. The ligand field parameters have been evaluated for Cu(II, Ni(II, Co(II, Mn(II and Fe(III complexes which suggest an octahedral geometry for each of them. The magnetic moment and spectral data suggest the dimeric nature of Mn(II complexes with octahedral geometry. The fungicidal activities of the ligands and their metal complexes have been screened in vitro against Aspergillus niger and the percentage inhibition of the metal complexes is found to be increased considerably then that of their corresponding ligands and the order is Cu>Ni>Fe>Mn>Co.

  8. Spectral characterization, molecular modeling and antimicrobial studies on hydrazone metal complexes of 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)dione and S-methyl dithiocarbazate.

    Science.gov (United States)

    Taha, Ali; Emara, Adel A A; Mashaly, Mahmoud M; Adly, Omima M I

    2014-09-15

    Metal complexes of copper(II), nickel(II), cobalt(II), oxovanadium(IV), chromium(III) and cadmium(II) with a new bridged ONS dibasic tridentate hydrazone (H2L) derived from 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)-dione with S-methyl dithiocarbazate have been synthesized and characterized by elemental analysis, molar conductance, magnetic susceptibility measurements, spectral (infrared, electronic, mass, 1H NMR and ESR) studies as well as thermal gravimetric analysis (TGA). The synthesized complexes have dimeric structures with the general formula [ML(NO3)m(H2O)x]2·nH2O·zMeOH, L=dianion of the hydrazone, m=0-1, x=0-2, n=0-4 and z=0-1. The metal complexes exhibited square planar, tetrahedral and octahedral geometrical arrangements, the molar conductivity data indicates that all complexes are neutral. The Coats-Redfern equation was used to calculate the kinetic and thermodynamic parameters for the different thermal decomposition stages of some complexes. Structural parameters of the ligand and its metal complexes have been theoretically computed on the basis of semiempirical PM3 level and the results were correlated with their experimental data. Antibacterial activities of the free ligand and its metal complexes were screened against various organisms.

  9. Synthesis and dual D2 and 5-HT1A receptor binding affinities of 5-piperidinyl and 5-piperazinyl-1H-benzo[d]imidazol-2(3H)-ones.

    Science.gov (United States)

    Ullah, Nisar

    2014-04-01

    A series of new 5-piperidinyl and 5-piperazinyl-1H-benzo[d]imidazol-2(3H)-ones have been synthesized and evaluated for dual D2 and 5-HT1A receptor binding affinities. The synthesized ligands are structurally related to bifeprunox, a potential atypical antipsychotic, having potent D2 receptor antagonist and 5-HT1A receptor agonist properties. The Suzuki-Miyaura reaction of cyclic vinyl boronate with appropriate aryl halide yielded arylpiperidine, which was eventually transformed to piperidinyl-1H-benzo[d]imidazol-2(3H)-one. The reductive amination of the latter with appropriate biarylaldehdyes rendered the synthesis of 5-piperidinyl-1H-benzo[d]imidazol-2(3H)-ones. Likewise, the Buchwald-Hartwig coupling reactions of 1-boc-piperazine with appropriate aryl halide and subsequent removal of the boc group rendered arylpiperazine. The reductive amination of the latter with appropriate biarylaldehdyes accomplished the synthesis of 5-piperazinyl-1H-benzo[d]imidazol-2(3H)-ones. The structure-activity relationship studies showed that cyclopentenylpyridine and cyclopentenylbenzyl groups contribute significantly to the dual D2 and 5-HT1A receptor binding affinities of these compounds.

  10. Um estudo teórico de propriedades moleculares em complexos de hidrogênio trimoleculares C2H4···2HF, C2H2···2HF e C3h6···2HF A theoretical study of molecular properties of C2H4···2HF, C2H2···2HF AND C3H6···2HF trimolecular hydrogen-bonded complexes

    Directory of Open Access Journals (Sweden)

    Boaz G. Oliveira

    2008-01-01

    Full Text Available We present a theoretical study of molecular properties in C2H4···2HF, C2H2···2HF and C3H6···2HF trimolecular hydrogen-bonded complexes. From B3LYP/6-311++G(d,p calculations, the most important structural deformations are related to the C=C (C2H4, C≡C (C2H2, C-C (C3H6 and HF bond lengths. According to the Bader's atoms in molecules and CHELPG calculations, it was identified a tertiary interaction between the fluorine atom of the second hydrofluoric acid molecule and hydrogen atoms of the ethylene and acetylene within the C2H4···2HF and C2H2···2HF complexes, respectively. Additionally, the evaluation of the infrared spectrum characterized the new vibrational modes and bathochromic effect of the HF molecules.

  11. Oxidative cross-coupling of pyridine N-oxides and ethers between C(sp(2))-H/C(sp(3))-H bonds under transition-metal-free conditions.

    Science.gov (United States)

    Sun, Wei; Xie, Zuguang; Liu, Jie; Wang, Lei

    2015-04-21

    A novel and efficient method based on the cross-coupling reactions of pyridine N-oxides with ethers between C(sp(2))-H/C(sp(3))-H bonds in the presence of TBHP was developed. The strategy provides an alternative approach to the pyridine moiety under transition-metal-free conditions.

  12. Hydrogen isotope systematics in C3 and C4 saltmarsh plants: the importance of biochemical processes in controlling interspecies variation in n-alkane 2H/1H composition

    Science.gov (United States)

    Eley, Y.; Pedentchouk, N.

    2013-12-01

    Palaeohydrological studies have increasingly utilised the 2H/1H composition of leaf wax n-alkyl lipids to extract information from the geological record. Interpretation of the sedimentary biomarker δ2H signal, however, requires detailed understanding of the mechanisms controlling hydrogen isotope fractionation between source water and n-alkyl lipids (ɛl/w). The existence of large ranges in published n-alkyl δ2H and ɛl/w among modern plant species growing at a single location suggests that the lipid signal incorporated into the sedimentary record could be sensitive to relatively small-scale changes in vegetation assemblages. The mechanisms responsible for these interspecies differences are currently poorly constrained. Previous research has had limited success explaining n-alkyl δ2H by reference to physical processes controlling the movement of water inside/outside and within the leaf, while the relative importance of biochemical processes remains largely unexplored. This project aims to identify the mechanisms controlling interspecies variation in n-alkane 2H/1H among a range of C3 and C4 plants from a Norfolk saltmarsh in the UK. To distinguish between environmental, physical and biochemical controls, we conducted 2H/1H analysis of soil, xylem, and leaf waters and n-alkanes (i) across multiple sampling sites within the marsh, (ii) throughout the 2012 growth season, and (iii) at different times of the day. We also measured the 2H/1H of chloroplast phytol in 7 samples collected at the end of 2012. Leaf wax n-alkane δ2H varied among the sampled species by over 100‰ throughout the 2012 growth season. Environmental processes that could influence control source water 2H/1H did not fully account for this interspecies variation - soil water 2H/1H varied by only 35‰ with marsh sub-environment and exhibited site-specific seasonal shifts by no more than 31‰. Maximum interspecies variation in xylem water was 38‰, while leaf waters differed by only 29‰. We

  13. Hydrothermal synthesis, electrochemical properties and calculation of complex { Cu[ PHBA ]2 ( H2O)3 } (H2O)3%配合物{Cu[PHBA]2(H2O)3}(H2O)3的水热合成、晶体结构、电化学分析及量化计算

    Institute of Scientific and Technical Information of China (English)

    刘雄祥; 李昶红

    2007-01-01

    在甲醇和水的混合溶剂中通过水热反应,以对羟基苯甲酸和4,4'-联吡啶为配体合成了配合物{Cu[PHBA]2(H2O)3}(H2O)3,并测定了配合物的晶体结构,该晶体属三斜晶系,空间群c2(1),晶胞参数为:a=2.4428(5)nm,b=1.14476(17)nm,c=0.72516(11)nm,α=β=γ=90.00°,V=2.0278(6)nm3,Dc=1.578g/cm3,Z=4,F(000)=1004.最终偏离因子R1=0.0304,wR2=0.0796.配合物中Cu(Ⅱ)离子与2个对羟基苯甲酸的2个羧基O原子及3个水分子中的3个氧原子配位,形成三角双锥结构,铜位于结构中心.结合晶体结构对配合物进行了电化学性质分析和量子化学计算.

  14. 8,8-Dimethyl-5-(4-methylphenyl-8,9-dihydropyrimido[4,5-b]quinoline-2,4,6(1H,3H,7H-trione N,N-dimethylformamide solvate

    Directory of Open Access Journals (Sweden)

    Daqing Shi

    2008-03-01

    Full Text Available The title compound, C20H19N3O3·C3H7NO, was synthesized by the reaction of 6-aminopyrimidine-2,4(1H,3H-dione and 4-methylbenzaldehyde with 5,5-dimethyl-1,3-cyclohexanedione in 1-butyl-3-methylimidazolium bromide at 363 K. The pyrimidine ring adopts a half-chair conformation while the six-membered ring fused to the pyridine ring adopts a skew-boat conformation. The dihedral angle between the pyridine ring and the attached benzene ring is 2.38(8°

  15. Narcissus tazetta lectin shows strong inhibitory effects against respiratory syncytial virus, influenza A (H1N1, H3N2, H5N1) and B viruses

    Indian Academy of Sciences (India)

    Linda S M Ooi; Wing-Shan Ho; Karry L K Ngai; Li Tian; Paul K S Chan; Samuel S M Sun; Vincent E C Ooi

    2010-03-01

    Amannose-binding lectin (Narcissus tazetta lectin [NTL]) with potent antiviral activity was isolated and purified from the bulbs of the Chinese daffodil Narcissus tazetta var. chinensis, using ion exchange chromatography on diethylaminoethyl (DEAE)-cellulose, affinity chromatography on mannose–agarose and fast protein liquid chromatography (FPLC)-gel filtration on Superose 12. The purified lectin was shown to have an apparent molecular mass of 26 kDa by gel filtration and 13 kDa by SDS–PAGE, indicating that it is probably a dimer with two identical subunits. The cDNA-derived amino acid sequence of NTL as determined by molecular cloning also reveals that NTL protein contains a mature polypeptide consisting of 105 amino acids and a C-terminal peptide extension. Three-dimensional modelling study demonstrated that the NTL primary polypeptide contains three subdomains, each with a conserved mannose-binding site. It shows a high homology of about 60%–80% similarity with the existing monocot mannose-binding lectins. NTL could significantly inhibit plaque formation by the human respiratory syncytial virus (RSV) with an IC50 of 2.30 g/ml and exhibit strong antiviral properties against influenza A (H1N1, H3N2, H5N1) and influenza B viruses with IC50 values ranging from 0.20 g/ml to 1.33 g/ml in a dose-dependent manner. It is worth noting that the modes of antiviral action of NTL against RSV and influenza A virus are significantly different. NTL is effective in the inhibition of RSV during the whole viral infection cycle, but the antiviral activity of NTL is mainly expressed at the early stage of the viral cycle of influenza A (H1N1) virus. NTL with a high selective index (SI=CC50/IC50 ≥ 141) resulting from its potent antiviral activity and low cytotoxicity demonstrates a potential for biotechnological development as an antiviral agent.

  16. In Vitro evaluation of antifungal activity of Bioactive Compound 2H-FURO [2,3-H]-1-Benzopyran-2-one against seed borne fungi of maize

    Directory of Open Access Journals (Sweden)

    B. Kiran

    2012-03-01

    Full Text Available Antifungal activity of bioactive compound 2HFuro[ 2,3-H]-1-benzopyran-2-one recorded a significant activity at 100-1000 ppm concentration against all the ten Aspergillus species tested. A. flavus recorded complete inhibition at 100 ppm concentration, A. niger at 500 ppm, A. fumigates at 600 ppm, A. flavus oryzae and A. flavus columnaris at 700 ppm respectively. A. ochraceous and A. flavipes recorded complete inhibition at 900 ppm concentration. Compared to synthetic fungicide Captan and Thiram at 2000ppm concentration. Minimum Inhibitory Concentration (MIC of bioactive compound was in the range of 100- 900ppm concentration against all the test fungi.

  17. Synthesis, Thermal Decomposition and Photochromic Kinetics of A Charge-transfer Salt (C_3H_5N_2H)_3 [PMo_(12)O_(40)]%电荷转移盐(C_3H_5N_2H)_3[PMo_(12)O_(40)]的合成与热分解及光致变色反应动力学

    Institute of Scientific and Technical Information of China (English)

    库宗军; 张忠海; 肖丽媛

    2010-01-01

    用磷钼酸与咪唑合成了一种新的杂多酸-有机电荷转移盐(C_3H_5N_2H)_3[PMo_(12)O_(40)].通过元素分析、红外光谱、固体漫反射光谱、电子自旋共振及热分析等测试技术对其进行了表征,用单扫描法(Achar法和Coats-Redfern法)对合成化合物的TG分析结果进行了非等温热分解动力学研究.推断结果表明,合成化合物的第1步热分解为球对称的三维扩散机理(n=2),其动力学方程为dα/dt=1.58×10~8[1-(1-α)~(1/3)]~(-1)(1-α)~(2/3)exp(-40 931.0/T),求得分解反应的表观活化能E=340.30 kJ/mol,指前因子A=1.05×10~8 s~(-1).标题化合物对紫外光具有光致变色性质,用固体漫反射光谱研究了其光致变色反应动力学.结果显示,其光致变色反应表现为一级或准一级动力学,速率常数k=9.80×10~(-5) s~(-1).

  18. Synthesis and Electrical and Gas Sensing Properties of Some 5-(Quinolinylmethylene-2-thioxodihydropyrimidine-4,6(1H,5H-dione and 5-(Quinolinylmethylenepyrimidine-2,4,6(1H,3H,5H-trione Derivatives

    Directory of Open Access Journals (Sweden)

    H. Kerim Beker

    2013-01-01

    Full Text Available Eight new 5-(quinolinylmethylenebarbituric acid derivatives were synthesized by the reaction of 1,3-dimethylbarbituric acid and 1,3-diethyl-2-thiobarbituric acid with quinoline-4-carboxaldehydes and several quinoline-2-carboxaldehydes via Knoevenagel condensation. The novel compounds were characterized by 1H NMR, 13C NMR, mass, IR, and UV-visible spectral data and elemental analyses. d.c. and a.c. conduction properties of the compounds were investigated in the frequency range of 40–105 Hz and temperature range 295–440 K. The d.c. results showed an activated conductivity dependence on temperature for all films. Obtained data reveal that a.c. conductivity obeys the relation and exponent is found to decrease by increasing temperature. The analysis of the a.c. conduction data showed that the CBH model is the dominant conduction mechanism for the electron transport in the films. Gas sensing properties of the films for the volatile organic compounds (VOCs were also investigated in the same temperature range. Maximum sensitivity to VOCs was observed at around 360 K for compound 6.

  19. Both water source and atmospheric water impact leaf wax n-alkane 2H/1H values of hydroponically grown angiosperm trees

    Science.gov (United States)

    Tipple, B. J.; Berke, M. A.; Hambach, B.; Roden, J. S.; Ehleringer, J. R.

    2013-12-01

    The extent to which both water source and leaf water 2H-enrichment affect the δ2H values of terrestrial plant leaf waxes is an area of active research as ecologists seek a mechanistic understanding of the environmental determinants of leaf wax isotope values before applying δ2H values of leaf waxes to reconstruct past hydrologic conditions. To elucidate the effects of both water source and atmospheric water vapor on δ2H values of leaf waxes for broad-leaved angiosperms, we analyzed hydrogen isotope ratios of high-molecular weight n-alkanes from two tree species that were grown throughout the spring and summer (five months) in a hydroponic system under controlled atmospheric conditions. Here, 12 subpopulations each of Populus fremontii and Betula occidentalis saplings were grown under one of six source different waters ranging in hydrogen isotope ratio values from -120 to +180 ‰ and under either 40 % or 75 % relative humidity conditions. We found n-alkane δ2H values of both species were linearly related to source water δ2H values with differences in slope associated with differing atmospheric humidity. A Craig-Gordon model was used to predict the δ2H values of leaf water and, by extension, n-alkane δ2H values under the range of growth conditions. The modeled leaf water values were found to be linearly related to observed n-alkane δ2H values with a statistically indistinguishable slope between the high and low humidity treatments. These leaf wax observations support a constant biosynthetic fractionation factor between evaporatively-enriched leaf water and n-alkanes for each species. However, we found the calculated biosynthetic fractionation between modeled leaf-water and n-alkane to be different between the two species. We submit that these dissimilarities were due to model inputs and not differences in the specific-species biochemistry. Nonetheless, these results are significant as they indicated that the δ2H value of atmospheric water vapor and

  20. Naturally Occurring Antibodies in Humans Can Neutralize a Variety of Influenza Virus Strains, Including H3, H1, H2, and H5 ▿ §

    Science.gov (United States)

    Ohshima, Nobuko; Iba, Yoshitaka; Kubota-Koketsu, Ritsuko; Asano, Yoshizo; Okuno, Yoshinobu; Kurosawa, Yoshikazu

    2011-01-01

    Influenza A viruses are classified into 16 subtypes according to the serotypes of hemagglutinin (HA). It is generally thought that neutralizing antibodies (Abs) are not broadly cross-reactive among HA subtypes. We examined the repertoire of neutralizing Abs against influenza viruses in humans. B lymphocytes were collected from donors by apheresis, and Ab libraries were constructed by using phage-display technology. Anti-HA clones were isolated by screening with H3N2 viruses. Their binding activity was examined, and four kinds of Abs showing broad strain specificity were identified from one donor. Two of the Abs, F045-092 and F026-427, were extensively analyzed. They neutralized not only H3N2 but also H1N1, H2N2, and H5N1 viruses, although the activities were largely varied. Flow cytometry suggested that they have the ability to bind to HA and HA1 artificially expressed on the cell surface. They show hemagglutination inhibition activity and do not compete with C179, an Ab thought to bind to the stalk region. F045-092 competes with Abs that recognize sites A and B for binding to HA. Furthermore, the serine at residue 136 in site A could be a part of the epitope. Thus, it is likely that F045-092 and F026-427 bind to a conserved epitope in the head region formed by HA1. Interestingly, while the VH1-69 gene can encode MAbs against the HA stem that are group 1 specific, F045-092 and its relatives that recognize the head region also use VH1-69. The possible epitope recognized by these clones is discussed. PMID:21865387

  1. Predicting leaf wax n-alkane 2H/1H ratios: controlled water source and humidity experiments with hydroponically grown trees confirm predictions of Craig-Gordon model.

    Science.gov (United States)

    Tipple, Brett J; Berke, Melissa A; Hambach, Bastian; Roden, John S; Ehleringer, James R

    2015-06-01

    The extent to which both water source and atmospheric humidity affect δ(2)H values of terrestrial plant leaf waxes will affect the interpretations of δ(2)H variation of leaf waxes as a proxy for hydrological conditions. To elucidate the effects of these parameters, we conducted a long-term experiment in which we grew two tree species, Populus fremontii and Betula occidentalis, hydroponically under combinations of six isotopically distinct waters and two different atmospheric humidities. We observed that leaf n-alkane δ(2)H values of both species were linearly related to source water δ(2)H values, but with slope differences associated with differing humidities. When a modified version of the Craig-Gordon model incorporating plant factors was used to predict the δ(2)H values of leaf water, all modelled leaf water values fit the same linear relationship with n-alkane δ(2)H values. These observations suggested a relatively constant biosynthetic fractionation factor between leaf water and n-alkanes. However, our calculations indicated a small difference in the biosynthetic fractionation factor between the two species, consistent with small differences calculated for species in other studies. At present, it remains unclear if these apparent interspecies differences in biosynthetic fractionation reflect species-specific biochemistry or a common biosynthetic fractionation factor with insufficient model parameterization.

  2. Isolation and structures of sulfonium salts derived from thioethers: [{o-C(6)H(4)(CH(2)SMe)(2)}H][NbF(6)] and [{[9]aneS(3)}H][NbF(6)].

    Science.gov (United States)

    Jura, Marek; Levason, William; Reid, Gillian; Webster, Michael

    2009-10-07

    Two very unusual sulfonium salts, [{o-C(6)H(4)(CH(2)SMe)(2)}H][NbF(6)] and [{[9]aneS(3)}H][NbF(6)], obtained from reaction of the thioethers with NbF(5) in CH(2)Cl(2) solution, are reported and their structures described; the eight-coordinate tetrafluoro Nb(v) cation of the dithioether is obtained from the same reaction.

  3. Low-energy SiC2H6+ and SiC3H9+ ion beam productions by the mass-selection of fragments produced from hexamethyldisilane for SiC film formations

    Directory of Open Access Journals (Sweden)

    Satoru Yoshimura

    2016-12-01

    Full Text Available We have been attempting to produce low-energy ion beams from fragments produced through the decomposition of hexamethyldisilane (HMD for silicon carbide (SiC film formations. We mass-selected SiC2H6+ and SiC3H9+ ions from fragments produced from HMD, and finally produced low-energy SiC2H6+ and SiC3H9+ ion beams. The ion energy was approximately 100 eV. Then, the ion beams were irradiated to Si(100 substrates. The temperature of the Si substrate was 800°C during the ion irradiation. The X-ray diffraction and Raman spectroscopy of the substrates obtained following SiC2H6+ ion irradiation demonstrated the occurrence of 3C-SiC deposition. On the other hand, the film deposited by the irradiation of SiC3H9+ ions included diamond-like carbon in addition to 3C-SiC.

  4. One-pot synthesis and antibacterial activities of novel 1H-pyridazino[1,2-a]indazole-1,6,9(2H,11H)-triones.

    Science.gov (United States)

    Sayyafi, Maryam; Soorki, Ali Abolhasani; Bazgir, Ayoob

    2008-09-01

    Synthesis of novel 1H-pyridazino[1,2-a]indazole-1,6,9(2H,11H)-triones using one-pot, three components reaction of 1,2-dihydropyridazine-3,6-dione, dimedone and aldehydes under solvent-free conditions has been reported. These products were evaluated in vitro for their antibacterial activities.

  5. Simultaneous Determination of the 2H/1H, 17O/16O, and 18O/16O Isotope Abundance Ratios in Water by Means of Laser Spectrometry

    NARCIS (Netherlands)

    Kerstel, E.R.Th.; Trigt, R. van; Dam, N.J.; Reuss, J.; Meijer, H.A.J.

    1999-01-01

    We demonstrate the first successful application of infrared laser spectrometry to the accurate, simultaneous determination of the relative H-2/H-1, O-17/O-16, and O-18/O-16 isotope abundance ratios in water. The method uses a narrow Line width color center laser to record the direct absorption spect

  6. Identification and correction of spectral contamination in 2H/1H and 18O/16O measured in leaf, stem, and soil water.

    Science.gov (United States)

    Schultz, Natalie M; Griffis, Timothy J; Lee, Xuhui; Baker, John M

    2011-11-15

    Plant water extracts typically contain organic materials that may cause spectral interference when using isotope ratio infrared spectroscopy (IRIS), resulting in errors in the measured isotope ratios. Manufacturers of IRIS instruments have developed post-processing software to identify the degree of contamination in water samples, and potentially correct the isotope ratios of water with known contaminants. Here, the correction method proposed by an IRIS manufacturer, Los Gatos Research, Inc., was employed and the results were compared with those obtained from isotope ratio mass spectrometry (IRMS). Deionized water was spiked with methanol and ethanol to create correction curves for δ(18)O and δ(2)H. The contamination effects of different sample types (leaf, stem, soil) and different species from agricultural fields, grasslands, and forests were compared. The average corrections in leaf samples ranged from 0.35 to 15.73‰ for δ(2)H and 0.28 to 9.27‰ for δ(18)O. The average corrections in stem samples ranged from 1.17 to 13.70‰ for δ(2)H and 0.47 to 7.97‰ for δ(18)O. There was no contamination observed in soil water. Cleaning plant samples with activated charcoal had minimal effects on the degree of spectral contamination, reducing the corrections, by on average, 0.44‰ for δ(2)H and 0.25‰ for δ(18)O. The correction method eliminated the discrepancies between IRMS and IRIS for δ(18)O, and greatly reduced the discrepancies for δ(2)H. The mean differences in isotope ratios between IRMS and the corrected IRIS method were 0.18‰ for δ(18)O, and -3.39‰ for δ(2)H. The inability to create an ethanol correction curve for δ(2)H probably caused the larger discrepancies. We conclude that ethanol and methanol are the primary compounds causing interference in IRIS analyzers, and that each individual analyzer will probably require customized correction curves.

  7. Quantum mechanical and spectroscopic (FT-IR, FT-Raman,1H,13C NMR, UV-Vis) studies, NBO, NLO, HOMO, LUMO and Fukui function analysis of 5-Methoxy-1H-benzo[d]imidazole-2(3H)-thione by DFT studies

    Science.gov (United States)

    Pandey, Manju; Muthu, S.; Nanje Gowda, N. M.

    2017-02-01

    Theoretical analysis of the molecular structure, spectroscopic (FT-IR, FT-Raman, 1H, 13C NMR, UV-Vis) studies, and thermodynamic characteristics of 5-Methoxy-1H-benzo[d]imidazole-2(3H)-thione (5MBIT) molecule were done by DFT/B3LYP using 6-311++G(d, p) basis set. Theoretical parameters were compared with experimental data. The dipole moment (μ), polarizability (Δα) and first order hyperpolarizability (β) of the molecule were calculated. Thermodynamic properties, HOMO and LUMO energies were determined. Global reactivity parameters and Fukui function of the 5MBIT molecule were predicted.

  8. Synthesis of New 2-Halo-2-(1H-tetrazol-5-yl-2H-azirines via a Non-Classical Wittig Reaction

    Directory of Open Access Journals (Sweden)

    Ana L. Cardoso

    2015-12-01

    Full Text Available The synthesis and reactivity of tetrazol-5-yl-phosphorus ylides towards N-halosuccinimide/TMSN3 reagent systems was explored, opening the way to new haloazidoalkenes bearing a tetrazol-5-yl substituent. These compounds were obtained as single isomers, except in one case. X-ray crystal structures were determined for three derivatives, establishing that the non-classical Wittig reaction leads to the selective synthesis of haloazidoalkenes with (Z-configuration. The thermolysis of the haloazidoalkenes afforded new 2-halo-2-(tetrazol-5-yl-2H-azirines in high yields. Thus, the reported synthetic methodologies gave access to important building blocks in organic synthesis, vinyl tetrazoles and 2-halo-2-(tetrazol-5-yl-2H-azirine derivatives.

  9. NMS-P937, a 4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline derivative as potent and selective Polo-like kinase 1 inhibitor.

    Science.gov (United States)

    Beria, Italo; Bossi, Roberto T; Brasca, Maria Gabriella; Caruso, Michele; Ceccarelli, Walter; Fachin, Gabriele; Fasolini, Marina; Forte, Barbara; Fiorentini, Francesco; Pesenti, Enrico; Pezzetta, Daniele; Posteri, Helena; Scolaro, Alessandra; Re Depaolini, Stefania; Valsasina, Barbara

    2011-05-15

    As part of our drug discovery effort, we identified and developed 4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline derivatives as PLK1 inhibitors. We now report the optimization of this class that led to the identification of NMS-P937, a potent, selective and orally available PLK1 inhibitor. Also, in order to understand the source of PLK1 selectivity, we determined the crystal structure of PLK1 with NMS-P937. The compound was active in vivo in HCT116 xenograft model after oral administration and is presently in Phase I clinical trials evaluation.

  10. Study of E/Z isomerization of (arylamino)methylidenefuran-2(3H)-ones by (1) H, (13) C, (15) N spectroscopy and DFT calculations in different solvents.

    Science.gov (United States)

    Osipov, Alexander K; Anis'kov, Alexander A; Grinev, Vyacheslav S; Yegorova, Alevtina Yu

    2017-08-01

    The structure and configuration of the series of previously unknown arylaminomethylidenefuran-2(3H)-ones have been determined in solution by (1) H, (13) C, (15) N nuclear magnetic resonance spectroscopy including two-dimensional experiments such as (1) H─(1) H COSY, dqCOSY, (1) H─(13) C HSQC, (1) H─(13) C HMBC. It was found that synthesized substances exist as an equilibrium mixture of E- and Z-enamines in solution. It was established on the basis of density functional theory calculations that the exchange between the two push-pull enamines is a simple rotation around an exocyclic partial double bond that depends on the effect of the solvents. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  11. The {sup 3}He(e,e'p){sup 2}H and {sup 4}He(e,e'p){sup 3}H reactions at high momentum transfer

    Energy Technology Data Exchange (ETDEWEB)

    Ford, William P. [Old Dominion University, Norfolk, VA (United States); Thomas Jefferson National Accelerator Facility, Newport News, VA (United States); Schiavilla, Rocco [Old Dominion University, Norfolk, VA (United States); Thomas Jefferson National Accelerator Facility, Newport News, VA (United States); Van Orden, J. W. [Thomas Jefferson National Accelerator Facility, Newport News, VA (United States)

    2014-03-01

    We present updated calculations for observables in the processes {sup 3}He(e,e'p){sup 2}H, {sup 4}He(e,e'p){sup 3}H and {sup 4}He(e-vector, e'p-vector){sup 3}H. This update entails the implementation of improved nucleon-nucleon (NN) amplitudes to describe final state interactions (FSI) within a Glauber approximation and includes full spin-isospin dependence in the profile operator. In addition, an optical potential, which has also been updated since previous work, is utilized to treat FSI for the {sup 4}He(e,e'p){sup 3}H and {sup 4}He(e-vector, e'p-vector){sup 3}H reactions. The calculations are compared with experimental data and show good agreement between theory and experiment. Comparisons are made between the various approximations in the Glauber treatment, including model dependence due to the NN scattering amplitudes, rescattering contributions, and spin dependence. We also analyze the validity of the Glauber approximation at the kinematics the data is available, by comparing to the results obtained with the optical potential.

  12. Supramolecular assembly based on a heteropolyanion: Synthesis and crystal structure of Na3(H2O)6[Al(OH)6Mo6O18]$\\cdot$2H2O

    Indian Academy of Sciences (India)

    Vaddypally Shivaiah; Samar K Das

    2005-05-01

    Synthesis and structural characterization of a polyoxometalate compound Na3(H2O)6 [Al(OH)6Mo6O18]$\\cdot$2H2O (1) have been described. Compound 1 exhibits three-dimensional network structure in the solid state, which is assembled by Anderson-type heteropolyanions, [Al(OH)6Mo6O18]$_n^{3n-}$, as building blocks sharing sodium cations. 1 possesses ``sinuous" channels occupied by supramolecular water dimers as guests. Anderson anions, sodium-coordinated water and crystal water are additionally involved in an intricate hydrogen-bonding network in the crystal of 1.

  13. Multicomponent Biginelli's synthesis of 3,4-dihydropyrimidin-2(1H-ones promoted by SnCl2.2H2O

    Directory of Open Access Journals (Sweden)

    Russowsky Dennis

    2004-01-01

    Full Text Available The ability of SnCl2.2H2O as catalyst to promote the Biginelli three-component condensation reaction from a diversity of aromatic aldehydes, ethyl acetoacetate and urea or thiourea is described. The reaction was carried out in acetonitrile or ethanol as solvents in neutral media and represents an improvement of the classical Biginelli protocol and an advantage in comparison with FeCl3.6H2O, NiCl2.6H2O and CoCl2.6H2O which were used with HCl as co-catalyst. The synthesis of 3,4-dihydropyrimidinones was achieved in good to excelent yields.

  14. An efficient synthesis of 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one catalyzed by recyclable solid superacid SO42-/TiO2under grinding condition

    Institute of Scientific and Technical Information of China (English)

    Guo Liang Feng

    2010-01-01

    An efficient synthesis of symmetrical 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO42-/TiO2 under solvent-free conditions at room temperature by grinding,which provides an efficient route to the synthesis of symmetrical 2,2-bis(1H-indol-3-yl)-2H-acenaphthen-1-one.This procedure offers several advantages including solvent-free conditions,excellent yields of products,simple work-up as well as reuse of catalysts which makes it a useful and attractive protocol for the synthesis of these compounds.

  15. Copper-catalyzed domino synthesis of 2-imino-1H-imidazol-5(2H)-ones and quinoxalines involving C-C bond cleavage with a 1,3-dicarbonyl unit as a leaving group.

    Science.gov (United States)

    Yang, Yan; Ni, Fan; Shu, Wen-Ming; Wu, An-Xin

    2014-09-08

    Although 2-imino-1H-imidazol-5(2H)-ones have important biological activities in metabolism, their synthesis has rarely been investigated. Quinoxalines as "privileged scaffolds" in medicinal chemistry have been extensively investigated, but the development of novel and efficient synthetic methods remains very attractive. Herein, we have developed two copper-catalyzed domino reactions for the synthesis of 2-imino-1H-imidazol-5(2H)-ones and quinoxalines involving CC bond-cleavage with a 1,3-dicarbonyl unit as a leaving group. The domino sequence for the synthesis of 2-imino-1H-imidazol-5(2H)-ones includes aza-Michael addition, intramolecular cyclization, CC bond-cleavage, 1,2-rearrangement, and aerobic dehydrogenation reaction, whereas the domino sequence for the synthesis of quinoxalines includes aza-Michael addition, intramolecular cyclization, elimination reaction, and CC bond-cleavage reaction. The two domino reactions have significant advantages including high efficiency, mild reaction conditions, and high tolerance of various functional groups. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Sauna, sweat and science - quantifying the proportion of condensation water versus sweat using a stable water isotope ((2)H/(1)H and (18)O/(16)O) tracer experiment.

    Science.gov (United States)

    Zech, Michael; Bösel, Stefanie; Tuthorn, Mario; Benesch, Marianne; Dubbert, Maren; Cuntz, Matthias; Glaser, Bruno

    2015-01-01

    Most visitors of a sauna appreciate the heat pulse that is perceived when water is poured on the stones of a sauna stove. However, probably only few bathers are aware that this pleasant heat pulse is caused by latent heat being released onto our skin due to condensation of water vapour. In order to quantify the proportion of condensation water versus sweat to dripping water of test persons we conducted sauna experiments using isotopically labelled (δ(18)O and δ(2)H) thrown water as tracer. This allows differentiating between 'pure sweat' and 'condensation water'. Two ways of isotope mass balance calculations were applied and yielded similar results for both water isotopes. Accordingly, condensation contributed considerably to dripping water with mean proportions of 52 ± 12 and 54 ± 7% in a sauna experiment in winter semester 2011/12 and 30 ± 13 and 33 ± 6% in a sauna experiment in winter semester 2012/13, respectively, depending on the way of calculating the isotope mass balance. It can be concluded from the results of our dual isotope labelling sauna experiment that it is not all about sweat in the sauna.

  17. Evaluation of the Sealed-tube Low-temperature Combustion Method for the 13C/12C and 2H/1H Ratio Determinations of Cellulose Nitrate

    Institute of Scientific and Technical Information of China (English)

    AUCOUR A.-M

    2001-01-01

    Traditionalluy+suggested combusion time of 1 h at 550℃ withthe sealed-tube combustion method for deternining the 13C/12C ratio of cellulose nitrate or other nitrogen-containing components could produce large negative deviation up to 1%o.Three types of cellulose are used to ascertain possible causes.The presence of nitrous oxide (N2O) formed during combus tion is most likely responsible for this deviation. Prolongation of the combustion time (at least 5 h at 550℃) and intimate coatact between copper oxide and organic matter can greatly improve the analysis precision and effectively reduce this devi ation to an acceptable level. Regardless of scattered carbon isotope data, hydrogen isotope data are all reproducible within 2‰ when this method is coupled with the high temperaure uranium reduction method. Thus, care should be taken for deternining carbon and nitrogen isotope com,positions of nitrogen-conaining substances using the low temperature sealedtube combustion method.

  18. Synthesis of some N-substituted aminoalkanol derivatives of 5,8-dimethyl-3b,9-epoxy-3a,4,5,6,7,8,9,9a-octahydro-1H-benzo[e]isoindole-1,3(2H)-dione and 6,7-dimethyl-4,9-epoxy-3a,4,5,8,9,9a-hexahydro-1H-benzo[f]isoindole-1,3(2H)-dione with an expected b-adrenolytic activity.

    Science.gov (United States)

    Kossakowski, Jerzy; Raszkiewicz, Aldona

    2004-12-01

    Pindolol and propranolol are used in the treatment of cardiovascular diseases, including hypotension or hypertension and antiarrythmic. Moreover, in the light of current 5-HT receptors classification it is known the mentioned drugs possess high 5-HT1A/5-HT1B affinity. It allows to establish two ways of researches. Department of Medicinal Chemistry of Medical University of Warsaw reports on synthesis of new compounds, analogues of Propranolol and Pindolol. A series of 5,8-dimethyl-3b,9-epoxy-3a,4,5,6,7,8,9,9a-octahydro-1H-benzo[e]isoindole-1,3(2H)-dione and 6,7-dimethyl-4,9-epoxy-3a,4,5,8,9,9a-hexahydro-1H-benzo[f]isoindole-1,3(2H)-dione have been designed with oxygen bridged rings. This property provides pharmacological activity increasing and toxicity decreasing.

  19. Peptide-nucleic acids (PNAs) with pyrimido[4,5-d]pyrimidine-2,4,5,7-(1H,3H,6H,8H)-tetraone (PPT) as a universal base: their synthesis and binding affinity for oligodeoxyribonucleotides.

    Science.gov (United States)

    Hirano, Taisuke; Kuroda, Kenji; Kataoka, Masanori; Hayakawa, Yoshihiro

    2009-07-21

    Peptide-nucleic acids (PNAs) including pyrimido[4,5-d]pyrimidine-2,4,5,7-(1H,3H,6H,8H)-tetraone (PPT) as a nucleobase were synthesized, and their binding affinity for the complementary oligodeoxyribonucleotides was investigated. We found that PNAs with one or two PPT(s) and natural nucleobases (i.e., adenine, cytosine, guanine, or thymine) have excellent binding affinity for oligodeoxyribonucleotides with complementary bases at the positions facing the natural nucleobases, and with adenine, cytosine, guanine, and thymine at the positions opposite PPT in PNAs. The binding affinity of the PPT-containing PNA is higher than or comparable to that of a PNA consisting of all complementary natural nucleobases, viz. a PNA with a suitable natural nucleobase in place of PPT in the PPT-containing PNA. Consequently, it was concluded that PPT serves as a useful universal base that can recognize all natural nucleobases.

  20. Characterization of protein/ligand interactions by {sup 1}H/{sup 3}H exchange: application to the hAsf{sup 1}/ histone H{sup 3} complex; Caracterisation des interactions proteine / ligand par echange {sup 1}H/{sup 3}H: application au complexe entre la proteine hAsf{sup 1} et l'histone H{sup 3}

    Energy Technology Data Exchange (ETDEWEB)

    Mousseau, G

    2007-05-15

    In the first chapter will be exposed the main current methods of identification to high debit of the interactions protein-protein. Then the methods allowing to characterize the surfaces of interaction or to determine the structures of the complexes will be listed by discussing the main advantages and the inconveniences. Our approach of characterization of the zones of interaction protein-protein is a method of 'foot-printing' 1, based on the identification and radicals' quantification formed on the residues of proteins accessible to the water. The second chapter will so discuss the development of this method of radical identification using the atom of tritium as radioactive label. Our approach will finally be validated in the third chapter by applying it to the characterization of amino acids involved in the interaction enter the human protein anti silencing factor 1 (hAsf11-156) and a fragment of the histone H{sup 3}. (N.C.)

  1. Organotin(IV) carboxylates based on 2-(1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)acetic acid: Syntheses, crystal structures, luminescent properties and antitumor activities

    Science.gov (United States)

    Xiao, Xiao; Liang, Jingwen; Xie, Jingyi; Liu, Xin; Zhu, Dongsheng; Dong, Yuan

    2017-10-01

    Organotin carboxylates based on an amide carboxylic acid 2-(1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)acetic acid (HL): [(Bn2Sn)2O2L]2·2C6H6 (1) (Bn = benzyl group) and (Ph2Sn)(L)2 (2) were synthesized and characterized by elemental analysis, IR, 1H, 13C, 119Sn NMR spectroscopy and X-ray crystallography diffraction analysis. Complex 1 is dimeric carboxylate tetraorganodistannoxane and show a ;ladder-like; molecular structure. Complex 2 is a dialkyltin carboxylate monomer possessing crystallographically imposed two-fold symmetry. Ligand in 1 and 2 adopts unidentate and bidentate coordination respectively. Both 1 and 2 form 1D, 2D and 3D supramolecular organizations in the solid state mediated through Csbnd H⋯O and π⋯π interactions which are discussed in detail. The luminescent properties and preliminary antitumor activities about this series of complexes were also studied.

  2. A three-dimensional structure of vanadium malonate: synthesis, characterization and X-ray structure of [Na 2VO(C 3H 2O 4) 2(H 2O) 2] n

    Science.gov (United States)

    Zhang, Quan-Zheng; Lu, Can-Zhong; Yang, Wen-Bin; Chen, Shu-Mei; Yu, Ya-Qin

    2004-05-01

    A three-dimensional structure [Na 2VO(C 3H 2O 4) 2(H 2O) 2] n was synthesized from the aqueous solution of V 2O 5, malonic acid and HCl. The compound crystallizes in orthorhombic system, space group C222 1 with a=7.2472(9) Å, b=15.9465(2) Å, c=10.3672(1) Å, V=1198.1(3) Å 3, Z=4, and R1=0.0242 for 1027 observed reflections. Single crystal X-ray diffraction reveals that the vanadium atom is coordinated by six oxygen atoms in an octahedral geometry. It is more interesting that one sodium ion is coordinated by two μ 3-OH 2 and six carboxyl oxygen atoms, which exhibits an unusual coordination mode. The malonato-vanadium units are linked up by two sodium ions to an extended network

  3. Synthesis and crystal structure of an organic-inorganic complex [Cu(DMF)3(H2O)2]2[SiMo12O40]·2H2O

    Institute of Scientific and Technical Information of China (English)

    WANG Jingping; DU Xiaodi; DUAN Xianying; NIU Jingyang

    2007-01-01

    The synthesis and crystal structure of an polyoxometalate-based organic-inorganic complex [Cu(DMF)3(H2O)2]2[SiMo12O40]·2H2O (DMF = N, N-dimethyl formamide) is described in this article. It was characterized using elemental analysis, thermal analysis, infrared, ultraviolet, and electron spin resonance spectroscopic studies. The X-ray crystallography analysis showed that the copper centers are pentacoordinated to show the square pyramidal geometry, and the polyanion [SiMo12O40]4- which is semi-coordinated to the copper(Ⅱ) centers prevents the existence of a sixth ligand. In addition, the intracationic hydrogen interaction enhanced the stability of the copper coordination cation.

  4. Epitaxy of Si1- x C x via ultrahigh-vacuum chemical vapor deposition using Si2H6, Si3H8, or Si4H10 as Si precursors

    Science.gov (United States)

    Koo, Sangmo; Jang, Hyunchul; Ko, Dae-Hong

    2017-09-01

    In this study, disilane (Si2H6), trisilane (Si3H8), and tetrasilane (Si4H10) were used as Si precursors for the growth of Si1- x C x epilayers, and the growth properties of the layers were compared. The use of a higher-order silane significantly increased the growth rates of the Si1- x C x epilayers at a processing temperature of 650 °C. In addition, a higher growth rate realized by using a higher-order silane promoted an increase in the substitutional carbon concentration in the Si1- x C x epilayers owing to the additional injection of a C-source gas (SiH3CH3) and the incorporation of C atoms into substitutional sites. The differences in growth properties between Si precursors were explained on the basis of reaction mechanisms.

  5. Synthesis and antibacterial activity of a new series of 3-[3-(substituted phenyl)-1-isonicotinoyl-1H-pyrazol-5-yl]-2H-chromen-2-one derivatives.

    Science.gov (United States)

    Aragade, Prashant; Maddi, Veeresh; Khode, Suresh; Palkar, Mahesh; Ronad, Pradeepkumar; Mamledesai, Shivalingarao; Satyanarayana, Darbhamulla

    2009-06-01

    A novel series of 3-[3-(substituted phenyl)-1-isonicotinoyl-1H-pyrazol-5-yl]-2H-chromen-2-one derivatives 4a-k have been synthesized by the reaction of 3-[2,3-dibromo-3-(substituted phenyl) propanoyl]-2H-chromen-2-one 3a-k and isonicotinic acid hydrazide in the presence of triethylamine in absolute ethanol, characterized by spectral data and screened for their in-vitro antibacterial activity against Gram-positive and Gram-negative bacteria. Among the series, compounds 4e, 4i, and 4k displayed an encouraging antibacterial activity profile as compared to the reference drug ampicillin against tested bacterial strains.

  6. Synthesis and anti-microbial activity of new (1-alkyl-1H-1,2,3-triazol-4-ylmethyl-2H-chromene-3-carboxylates: A click chemistry approach

    Directory of Open Access Journals (Sweden)

    M. Koteswara Reddy

    2015-07-01

    Full Text Available A series of new 1,4 disubstituted (1-alkyl-1H-1,2,3-triazol-4-ylmethyl-2H-chromene-3-carboxylates (4ai–4eiii have been efficiently synthesized in moderate to excellent yields by the 1,3 dipolar cycloaddition between 2-propynyl-2H-chromene-3-carboxylates 3a–e and various alkyl azides under Cu(I catalyzed conditions. The structures of the synthesized compounds are established based on IR, NMR, MASS Spectrometric methods and elemental analyses. The antibacterial and antifungal activities of synthesized compounds were evaluated. Compounds 4biii, 4ei, 4dii, 4ai, 4aii, 4bii showed good activity against bacterial strains and the compounds 4bi, 4eii against fungal strains.

  7. Measurements of GEn/GMn from the ^2H(vec{e},e'vec{n})^1H Reaction to Q^2=1.45 (GeV/c)^2

    CERN Document Server

    Madey, R; Taylor, S; Plaster, B; Aghalaryan, A; Crouse, E; MacLachlan, G; Tajima, S; Tireman, W; Chen Yu Yan; Ahmidouch, A; Anderson, B D; Arenhövel, H; Asaturyan, R; Baker, O; Baldwin, A R; Barkhuff, D; Breuer, H; Carlini, R; Christy, E; Churchwell, S; Cole, L; Danagulyan, S; Day, D; Eden, T; Elaasar, M E; Ent, R; Farkhondeh, M; Fenker, H; Finn, J M; Gan, L; Garrow, K; Gueye, P; Howell, C R; Hu, B; Jones, M K; Kelly, J J; Keppel, C E; Khandaker, M; Kim, W Y; Kowalski, S; Lai, A; Lung, A; Mack, D; Manley, D M; Markowitz, P; Mitchell, J; Mkrtchyan, H G; Opper, A K; Perdrisat, C F; Punjabi, V; Raue, B A; Reichelt, T; Reinhold, J; Roche, J; Sato, Y; Savvinov, N; Semenova, I A; Seo, W; Simicevic, N; Smith, G; Stepanyan, S; Tadevosyan, V; Tang, L; Ulmer, P E; Vulcan, W; Watson, J W; Wells, S; Wesselmann, F; Wood, S; Chen Yan; Yang, S; Yuan, L; Zhang, W M; Zhu, H; Zhu, X

    2003-01-01

    We report new measurements of the ratio of the electric form factor to the magnetic form factor of the neutron, GEn/GMn, obtained via recoil polarimetry from the quasielastic ^2H(vec{e},e'vec{n})^1H reaction at Q^2 values of 0.45, 1.13, and 1.45 (GeV/c)^2 with relative statistical uncertainties of 7.6 and 8.4% at the two higher Q^2 points, which were not reached previously via polarization measurements. Scale and systematic uncertainties are small.

  8. Beam-energy dependence and updated test of the Trojan-horse nucleus invariance via a measurement of the 2H(d ,p )3H reaction at low energies

    Science.gov (United States)

    Li, Chengbo; Wen, Qungang; Tumino, A.; Fu, Yuanyong; Zhou, Jing; Zhou, Shuhua; Meng, Qiuying; Spitaleri, C.; Pizzone, R. G.; Lamia, L.

    2017-03-01

    The 2H(d ,p )3H bare nucleus astrophysical S (E ) factor has been measured indirectly at energies from about 500 keV down to several keV by means of the Trojan-horse method applied to the 2H(6Li,p t )4He quasifree reaction induced at 11 MeV. The obtained results are compared with direct data as well as with previous indirect investigation of the same binary reactions. It shows that the precision of S (E ) data in the low-energy range extracted via the same Trojan-horse nuclei [6Li=(d ⊕α )] becomes better when the incident energy of the virtual binary process decreases from high value down to the lower Gamow energy range, which near the zero-quasi-free-energy point. The very good agreement between data extracted from different Trojan-horse nuclei [6Li=(d ⊕α ) vs 3He=(d ⊕p )] gives a strong updated test for the independence of the binary indirect cross section on the chosen Trojan-horse nucleus at low energies.

  9. Electrochromic Type E-Paper Using Poly(1H-Thieno[3,4-d]Imidazol-2(3H)-One) Derivatives by a Novel Printing Fabrication Process

    Science.gov (United States)

    Kondo, Yoshiro; Tanabe, Hirofumi; Kudo, Hidetoshi; Nakano, Kirihiro; Otake, Tomiaki

    2011-01-01

    In this study, we report poly(1H-thieno[3,4-d]imidazol-2(3H)-one) (pTIO) derivatives for an electrochromic (EC) type e-paper and its novel printing fabrication process. pTIO is a kind of conductive polymer (CP) s which are known as one of the EC materials. The electrochromism of pTIO is unique, because its color in doped state is almost transparent (pale gray). A transparent state is required to show a white color in a see-through view of an EC type e-paper. An electrochromism of CP has a good memory effect which is applicable for e-paper. The corresponding monomers of CP are able to be polymerized with an electrochemical method, which be made good use of for the fabrication process of e-paper. pTIO derivatives are copolymerized with other pi-conjugated X unit, which adjusts the color of electrochromism. Finally, we fabricated a segment matrix EC display using pTIO derivatives by ink-jet printing. PMID:28824131

  10. Electrochromic Type E-Paper Using Poly(1H-Thieno[3,4-d]Imidazol-2(3H-One Derivatives by a Novel Printing Fabrication Process

    Directory of Open Access Journals (Sweden)

    Kirihiro Nakano

    2011-12-01

    Full Text Available In this study, we report poly(1H-thieno[3,4-d]imidazol-2(3H-one (pTIO derivatives for an electrochromic (EC type e-paper and its novel printing fabrication process. pTIO is a kind of conductive polymer (CP s which are known as one of the EC materials. The electrochromism of pTIO is unique, because its color in doped state is almost transparent (pale gray. A transparent state is required to show a white color in a see-through view of an EC type e-paper. An electrochromism of CP has a good memory effect which is applicable for e-paper. The corresponding monomers of CP are able to be polymerized with an electrochemical method, which be made good use of for the fabrication process of e-paper. pTIO derivatives are copolymerized with other pi-conjugated X unit, which adjusts the color of electrochromism. Finally, we fabricated a segment matrix EC display using pTIO derivatives by ink-jet printing.

  11. Corrosion inhibition of mild steel in 1M HCl by D-glucose derivatives of dihydropyrido [2,3-d:6,5-d′] dipyrimidine-2, 4, 6, 8(1H,3H, 5H,7H)-tetraone

    Science.gov (United States)

    Verma, Chandrabhan; Quraishi, M. A.; Kluza, K.; Makowska-Janusik, M.; Olasunkanmi, Lukman O.; Ebenso, Eno E.

    2017-01-01

    D-glucose derivatives of dihydropyrido-[2,3-d:6,5-d′]-dipyrimidine-2, 4, 6, 8(1H,3H, 5H,7H)-tetraone (GPHs) have been synthesized and investigated as corrosion inhibitors for mild steel in 1M HCl solution using gravimetric, electrochemical, surface, quantum chemical calculations and Monte Carlo simulations methods. The order of inhibition efficiencies is GPH-3 > GPH-2 > GPH-1. The results further showed that the inhibitor molecules with electron releasing (-OH, -OCH3) substituents exhibit higher efficiency than the parent molecule without any substituents. Polarization study suggests that the studied compounds are mixed-type but exhibited predominantly cathodic inhibitive effect. The adsorption of these compounds on mild steel surface obeyed the Langmuir adsorption isotherm. SEM, EDX and AFM analyses were used to confirm the inhibitive actions of the molecules on mild steel surface. Quantum chemical (QC) calculations and Monte Carlo (MC) simulations studies were undertaken to further corroborate the experimental results. PMID:28317849

  12. Corrosion inhibition of mild steel in 1M HCl by D-glucose derivatives of dihydropyrido [2,3-d:6,5-d‧] dipyrimidine-2, 4, 6, 8(1H,3H, 5H,7H)-tetraone

    Science.gov (United States)

    Verma, Chandrabhan; Quraishi, M. A.; Kluza, K.; Makowska-Janusik, M.; Olasunkanmi, Lukman O.; Ebenso, Eno E.

    2017-03-01

    D-glucose derivatives of dihydropyrido-[2,3-d:6,5-d‧]-dipyrimidine-2, 4, 6, 8(1H,3H, 5H,7H)-tetraone (GPHs) have been synthesized and investigated as corrosion inhibitors for mild steel in 1M HCl solution using gravimetric, electrochemical, surface, quantum chemical calculations and Monte Carlo simulations methods. The order of inhibition efficiencies is GPH-3 > GPH-2 > GPH-1. The results further showed that the inhibitor molecules with electron releasing (-OH, -OCH3) substituents exhibit higher efficiency than the parent molecule without any substituents. Polarization study suggests that the studied compounds are mixed-type but exhibited predominantly cathodic inhibitive effect. The adsorption of these compounds on mild steel surface obeyed the Langmuir adsorption isotherm. SEM, EDX and AFM analyses were used to confirm the inhibitive actions of the molecules on mild steel surface. Quantum chemical (QC) calculations and Monte Carlo (MC) simulations studies were undertaken to further corroborate the experimental results.

  13. Synthesis of opioidmimetics, 3-[H-Dmt-NH(CH(2))(m)]-6-[H-Dmt-NH(CH(2))(n)]-2(1H)-pyrazinones, and studies on structure-activity relationships.

    Science.gov (United States)

    Shiotani, Kimitaka; Miyazaki, Anna; Li, Tingyou; Tsuda, Yuko; Yokoi, Toshio; Ambo, Akihiro; Sasaki, Yusuke; Bryant, Sharon D; Jinsmaa, Yunden; Lazarus, Lawrence H; Okada, Yoshio

    2007-11-01

    Opioidmimetics containing 3-[H-Dmt-NH-(CH(2))(m)]-6-[H-Dmt-NH-(CH(2))(n)]-2(1H)-pyrazinone symmetric (m = n, 1-4) (1 - 4) and asymmetric (m, n = 1 - 4) aliphatic chains (5 - 16) were synthesized using dipeptidyl chloromethylketone intermediates. They had high mu-affinity (K(i)mu = 0.021 - 2.94 nM), delta-affinity (K(i)delta = 1.06 - 152.6 nM), and mu selectivity (K(i)delta/K(i)mu = 14 - 3,126). The opioidmimetics (1 - 16) exhibited mu agonism in proportion to their mu-receptor affinity. delta-Agonism was essentially lacking in the compounds except (4) and (16), and (1) and (2) indicated weak delta antagonism (pA(2) = 6.47 and 6.56, respectively). The data verify that a specific length of aliphatic linker is required between the Dmt pharmacophore and the pyrazinone ring to produce unique mu-opioid receptor ligands.

  14. Interaction Study of an Amorphous Solid Dispersion of Cyclosporin A in Poly-Alpha-Cyclodextrin with Model Membranes by 1H-, 2H-, 31P-NMR and Electron Spin Resonance

    Directory of Open Access Journals (Sweden)

    Jean-Claude Debouzy

    2014-01-01

    Full Text Available The properties of an amorphous solid dispersion of cyclosporine A (ASD prepared with the copolymer alpha cyclodextrin (POLYA and cyclosporine A (CYSP were investigated by 1H-NMR in solution and its membrane interactions were studied by 1H-NMR in small unilamellar vesicles and by 31P 2H NMR in phospholipidic dispersions of DMPC (dimyristoylphosphatidylcholine in comparison with those of POLYA and CYSP alone. 1H-NMR chemical shift variations showed that CYSP really interacts with POLYA, with possible adduct formation, dispersion in the solid matrix of the POLYA, and also complex formation. A coarse approach to the latter mechanism was tested using the continuous variations method, indicating an apparent 1 : 1 stoichiometry. Calculations gave an apparent association constant of log Ka = 4.5. A study of the interactions with phospholipidic dispersions of DMPC showed that only limited interactions occurred at the polar head group level (31P. Conversely, by comparison with the expected chain rigidification induced by CYSP, POLYA induced an increase in the fluidity of the layer while ASD formation led to these effects almost being overcome at 298 K. At higher temperature, while the effect of CYSP seems to vanish, a resulting global increase in chain fluidity was found in the presence of ASD.

  15. Synthesis and characterization of the open-framework barium bisphosphonate [Ba3(O3PCH2NH2CH2PO3)2(H2O)4].3H2O.

    Science.gov (United States)

    Bauer, Sebastian; Müller, Helen; Bein, Thomas; Stock, Norbert

    2005-12-12

    Following the strategy of using polyfunctional phosphonic acids for the synthesis of open-framework metal phosphonates, the phosphonocarboxylic acid (H2O3PCH2)2NCH2C6H4COOH was used in the hydrothermal synthesis of new Ba phosphonates. Its decomposition led to the first open-framework barium phosphonate [Ba3(O3PCH2NH2CH2PO3)2(H2O)4].3H2O. The synthesis was also successfully performed using iminobis(methylphosphonic acid), (H2O3PCH2)2NH, as a starting material, and the synthesis was optimized to obtain as a pure material. The reaction setup as well as the pH are the dominant parameters, and only a diffusion-controlled reaction led to the desired compound. The crystal structure was solved from single-crystal data: monoclinic; C2/c; a=2328.7(2), b=1359.95(7), and c=718.62(6) pm; beta=98.732(10) degrees ; V=2249.5(3)x10(6) pm3; Z=4; R1=0.036; and wR2=0.072 (all data). The structure of [Ba3(O3PCH2NH2CH2PO3)2(H2O)4].3H2O is built up from BaO8 and BaO10 polyhedra forming BaO chains and layers, respectively. These are connected to a three-dimensional metal-oxygen-metal framework with the iminobis(methylphosphonic acid) formally coating the inner walls of the pores. The one-dimensional pores (3.6x4 A) are filled with H2O molecules that can be thermally removed. Thermogravimetric investigations and temperature-dependent X-ray powder diffraction demonstrate the stability of the crystal structure up to 240 degrees C. The uptake of N,N-dimethylformamide and H2O by dehydrated samples is demonstrated. Furthermore, IR, Raman, and 31P magic-angle-spinning NMR data are also presented.

  16. Iridium complexes containing mesoionic C donors: selective C(sp3)-H versus C(sp2)-H bond activation, reactivity towards acids and bases, and catalytic oxidation of silanes and water.

    Science.gov (United States)

    Petronilho, Ana; Woods, James A; Mueller-Bunz, Helge; Bernhard, Stefan; Albrecht, Martin

    2014-11-24

    Metalation of a C2-methylated pyridylimidazolium salt with [IrCp*Cl2]2 affords either an ylidic complex, resulting from C(sp(3))-H bond activation of the C2-bound CH3 group if the metalation is performed in the presence of a base, such as AgO2 or Na2CO3, or a mesoionic complex via cyclometalation and thermally induced heterocyclic C(sp(2))-H bond activation, if the reaction is performed in the absence of a base. Similar cyclometalation and complex formation via C(sp(2))-H bond activation is observed when the heterocyclic ligand precursor consists of the analogous pyridyltriazolium salt, that is, when the metal bonding at the C2 position is blocked by a nitrogen rather than a methyl substituent. Despite the strongly mesoionic character of both the imidazolylidene and the triazolylidene, the former reacts rapidly with D(+) and undergoes isotope exchange at the heterocyclic C5 position, whereas the triazolylidene ligand is stable and only undergoes H/D exchange under basic conditions, where the imidazolylidene is essentially unreactive. The high stability of the Ir-C bond in aqueous solution over a broad pH range was exploited in catalytic water oxidation and silane oxidation. The catalytic hydrosilylation of ketones proceeds with turnover frequencies as high as 6,000 h(-1) with both the imidazolylidene and the triazolylidene system, whereas water oxidation is enhanced by the stronger donor properties of the imidazol-4-ylidene ligands and is more than three times faster than with the triazolylidene analogue. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. 阿西替尼中间体(E)-6-碘-3-(2-(吡啶-2-基)乙烯基)-1-(四氢-2H-吡喃-2-基)-1H-吲唑的合成研究%Study on Synthesis of (E)-6-Iodo-3-(2-(pyridine-2-yl)vinyl)-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole

    Institute of Scientific and Technical Information of China (English)

    孟凡星; 张诗缇; 蔡东; 贾云宏

    2015-01-01

    (E)-6-碘-3-(2-(吡啶-2-基)乙烯基)-1-(四氢-2H-吡喃-2-基)-1H-吲唑是阿西替尼的关键中间体,以6-硝基-1H-吲唑为起始原料,经过碘代、加成、偶联、还原、碘代得到目标化合物.探讨了用微波辐射加热偶联反应的问题,并对各步反应合成条件进行了优化.改进后工艺总收率达42.32%(6-硝基-1H-吲唑为原料计),收率比文献报道值提高近5%,目标化合物和各中间体经1HNMR和MS等确证结构.改进后的工艺降低了成本,简单可行,适合工业化生产.

  18. Characterization, molecular modeling and antimicrobial activity of metal complexes of tridentate Schiff base derived from 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)-dione and 2-aminophenol.

    Science.gov (United States)

    Adly, Omima M I

    2012-09-01

    Metal complexes of Ni(II), Co(II), Cd(II), VO(IV) and UO(2)(VI) as well as several Cu(II) salts, including Cl(-),NO(3)(-),AcO(-),ClO(4)(-) and SO(4)(-2) with a tridentate O(2)N donor Schiff base ligand (H(2)L), synthesized by condensation of 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)-dione with 2-aminophenol, were prepared and characterized on the basis of elemental analyses, spectral, magnetic, molar conductance and thermal gravimetric analysis. Square planar, tetrahedral and octahedral geometries have been assigned to the prepared complexes. Molecular parameters of the ligand and its metal complexes have been calculated and correlated with the experimental data, and the changes of bond lengths are linearly correlated with IR data. The antimicrobial activities of the synthesized compounds were tested in vitro against the sensitive organisms Staphylococcus aureus as Gram positive bacteria, Proteus vulgaris as Gram negative bacteria and Candida albicans as fungus strain, and the results are discussed.

  19. Characterization, molecular modeling and antimicrobial activity of metal complexes of tridentate Schiff base derived from 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)-dione and 2-aminophenol

    Science.gov (United States)

    Adly, Omima M. I.

    Metal complexes of Ni(II), Co(II), Cd(II), VO(IV) and UO2(VI) as well as several Cu(II) salts, including Cl,NO3-,AcO,ClO4- and SO4-2 with a tridentate O2N donor Schiff base ligand (H2L), synthesized by condensation of 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)-dione with 2-aminophenol, were prepared and characterized on the basis of elemental analyses, spectral, magnetic, molar conductance and thermal gravimetric analysis. Square planar, tetrahedral and octahedral geometries have been assigned to the prepared complexes. Molecular parameters of the ligand and its metal complexes have been calculated and correlated with the experimental data, and the changes of bond lengths are linearly correlated with IR data. The antimicrobial activities of the synthesized compounds were tested in vitro against the sensitive organisms Staphylococcus aureus as Gram positive bacteria, Proteus vulgaris as Gram negative bacteria and Candida albicans as fungus strain, and the results are discussed.

  20. Synthesis and biological evaluation of novel 5-alkyl-2-arylthio-6-((3,4-dihydroquinolin-1(2H)-yl)methyl)pyrimidin-4(3H)-ones as potent non-nucleoside HIV-1 reverse transcriptase inhibitors.

    Science.gov (United States)

    Zhang, Jing; Zhan, Peng; Wu, Jingde; Li, Zhenyu; Jiang, Yan; Ge, Weiying; Pannecouque, Christophe; De Clercq, Erik; Liu, Xinyong

    2011-07-15

    A series of novel S-DABO analogues of 5-alkyl-2-arylthio-6-((3,4-dihydroquinolin-1(2H)-yl)methyl)pyrimidin-4(3H)-ones were synthesized and evaluated as inhibitors of human immunodeficiency virus type-1 (HIV-1). Among them, the most potent HIV-1 inhibitors were compounds 6c1,6c6, and 6b1 (EC(50)=0.24 ± 0.05, 0.38 ± 0.13, 0.39 ± 0.05 μM, respectively), which possess improved or similar HIV-1 inhibitory activity compared with nevirapine (NVP) (EC(50)=0.21 μM) and delavirdine (DLV) (EC(50)=0.32 μM). None of these compounds were active against HIV-2 replication. Furthermore, enzyme inhibitory assays were performed with selected derivatives against HIV-1 wtRT, confirming that the main target of these compounds is the HIV-1 RT and these new S-DABOs are acting as NNRTIs. The preliminary structure-activity relationship (SAR) of these new congeners is discussed briefly and rationalized by docking studies.

  1. Molecular conformational analysis, reactivity, vibrational spectral analysis and molecular dynamics and docking studies of 6-chloro-5-isopropylpyrimidine-2,4(1H,3H)-dione, a potential precursor to bioactive agent

    Science.gov (United States)

    Al-Omary, Fatmah A. M.; Mary, Y. Sheena; Beegum, Shargina; Panicker, C. Yohannan; Al-Shehri, Mona M.; El-Emam, Ali A.; Armaković, Stevan; Armaković, Sanja J.; Van Alsenoy, C.

    2017-01-01

    FT-IR and FT-Raman spectra of 6-chloro-5-isopropylpyrimidine-2,4(1H,3H)-dione were recorded and analyzed. The vibrational wavenumbers were computed using DFT quantum chemical calculations and the data obtained from wavenumber calculations are used to assign the experimentally obtained bands. Potential energy distribution was done using GAR2PED software. The geometrical parameters of the title compound are in agreement with the XRD results. NBO analysis, frontier molecular orbital and first and second hyperpolarizability and molecular electrostatic potential results are also reported. The possible electrophile attacking sites of the title compound is identified using MEP surface plot study. Molecule sites prone to electrophilic attacks were identified using average local ionization energy surfaces, while further insight into the local reactivity properties of the title molecule has been gained by calculation of Fukui functions. Intra-molecular non-covalent interactions have been detected and visualized. Degradation properties based on autoxidation and hydrolysis have been investigated by calculation of bond dissociation energies and radial distribution functions, respectively. From the molecular docking study, the ligand binds at the active site of the substrate by weak non-covalent interactions and amino acids Leu89 forms alkyl interaction with the CH3 groups and Glu90 amino acid forms π-anion interaction with the pyrimidine ring and Thr369 and Ser366 amino acids form H-bond interaction with the Cdbnd O and NH group, respectively. From the conformational analysis, the calculated structures show that the C6C9C10 angle in the most stable form is about 8° smaller compared to the C8C9C10 angle, indicating a higher repulsive force between the (CH3)2HC- moiety and the chlorine atom due to the size of chlorine compared to oxygen atoms.

  2. Measurements of the neutron electric to magnetic form factor ratio GEn/GMn via the ^2H(\\vec{e},e'\\vec{n})^1H reaction to Q^2 = 1.45 (GeV/c)^2

    CERN Document Server

    Plaster, B; Aghalaryan, A; Crouse, E; MacLachlan, G; Tajima, S; Tireman, W; Ahmidouch, A; Anderson, B D; Arenhövel, H; Asaturyan, R; Baker, O K; Baldwin, A R; Barkhuff, D; Breuer, H; Carlini, R; Christy, E; Churchwell, S; Cole, L; Danagulyan, S; Day, D; Eden, T; Elaasar, M; Ent, R; Farkhondeh, M; Fenker, H; Finn, J M; Gan, L; Gasparian, A; Garrow, K; Gueye, P; Howell, C R; Hu, B; Jones, M K; Kelly, J J; Keppel, C; Khandaker, M; Kim, W Y; Kowalski, S; Lung, A; Mack, D; Madey, R; Manley, D M; Markowitz, P; Mitchell, J; Mkrtchyan, H; Opper, A K; Perdrisat, C; Punjabi, V; Raue, B A; Reichelt, T; Reinhold, J; Roche, J; Sato, Y; Savvinov, N; Semenova, I A; Seo, W; Simicevic, N; Smith, G; Stepanyan, S; Tadevosyan, V; Tang, L; Taylor, S; Ulmer, P E; Vulcan, W; Watson, J W; Wells, S; Wesselmann, F; Wood, S; Yan, C; Yang, S; Yuan, L; Zhang, W M; Zhu, H; Zhu, X

    2003-01-01

    We report values for the neutron electric to magnetic form factor ratio, GEn/GMn, deduced from measurements of the neutron's recoil polarization in the quasielastic 2H(\\vec{e},e'\\vec{n})1H reaction, at three Q^2 values of 0.45, 1.13, and 1.45 (GeV/c)^2. The data at Q^2 = 1.13 and 1.45 (GeV/c)^2 are the first direct experimental measurements of GEn employing polarization degrees of freedom in the Q^2 > 1 (GeV/c)^2 region and stand as the most precise determinations of GEn for all values of Q^2.

  3. CH4、CO2及CH4+C2H6+C3H8在纯水、SDS水溶液和含石英砂体系中水合物相平衡条件的测定%Measurements of Hydrate Equilibrium Conditions for CH4, CO2, and CH4+ C2H6 + C3H8 in Various Systems by Step-heating Method

    Institute of Scientific and Technical Information of China (English)

    陈立涛; 孙长宇; 陈光进; 聂运强; 孙占松; 刘延涛

    2009-01-01

    Phase equilibrium conditions of gas hydrate in several systems were measured by the step-heating method using the cylindrical transparent sapphire cell device. The experimental data for pure CH4or CO2 + deion-ized water systems showed good agreement with those in the literatures. This kind of method was then applied to CH4/CO2 + sodium dodecyl sulfate (SDS) aqueous solution, CH4/CO2+SDS aqueous solution+silica sand, and (CH4+C2H6+C3H8) gas mixture+SDS aqueous solution systems, where SDS was added to increase the hydrate formation rate without evident influence on the equilibrium conditions. The feasibility and reliability of the step-heating method, especially for porous media systems and gas mixtures systems were determined. The experimental data for CO2+silica sand data shows that the equilibrium pressure will change significantly when the particle size of silica sand is less than 96 μm. The formation equilibrium pressure was also measured by the reformation of hydrate.

  4. Synthesis and Crystal Structure of 5-[(1H-1,2,4-Triazol-1- yl)methyl]-4-(2,3-dimethoxybenzylideneamino)-2- 2H-1,2,4-triazole-3(4H)-thione Monohydrate

    Institute of Scientific and Technical Information of China (English)

    XU Liang-Zhong; SHANG Yu-Qing; YU Guan-Ping; LI Kai; SI Guo-Dong

    2006-01-01

    The title compound 5-[(1H-1,2,4-triazol-1-yl)methyl]-4-(2,3-dimethoxy-benzyli- deneamino)- 2H-1,2,4-triazole-3(4H)-thione monohydrate 4 has been synthesized by the treatment of 4-amino-3-(1,2,4-triazol-1-yl)-1H-1,2,4-triazole-5(4H)-thione 3 with 2,3-dimethoxybenzaldehyde. It crystallizes as a monohydrate in the triclinic system, space group P-1 with a = 8.147(2), b = 10.820(2), c = 10.835(2) (A), α = 73.770(6), β = 84.916(7), γ = 70.679(6)°, C14H17N7O3S, Mr = 363.41, V = 865.4(2) (A)3, Z = 2, Dc = 1.395 g/cm3, F(000) = 380, μ = 0.217 mm-1, the final R = 0.0400 and wR = 0.0975 for 3454 unique reflections. The dihedral angles made by the thione-substituted triazole ring with the other triazole ring and benzene ring are 74.92(3) and 14.81(2)°, respectively. There are some weak hydrogen bonds and C-H…π supramolecular interactions in the lattice, forming a three-dimensional network, which stabilizes the crystal structure.

  5. Synthesis, molecular modeling, thermal and spectral studies of metal complexes of hydrazone derived from 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)-dione and thiosemicarbazide.

    Science.gov (United States)

    Adly, Omima M I

    2011-09-01

    Metal complexes with the general formula [ML(H2O)(CH3OH)x]·nH2O·(CH3OH)y(NO3)z [M=Cu(II), Ni(II), Co(II), VO(IV), Cr(III), Cd(II), Zn(II) or UO2(VI); x=0-2; y=0,1; z=0,1; n=0-2, 6 and L=hydrazone (H2L) derived from condensation of thiosemicarbazide with 5-acetyl-4-hydroxy-2H-1,3-thiazine-2,6(3H)-dione. The synthesized ligand and its metal complexes have been characterized on the basis of elemental analyses, spectral and magnetic studies as well as thermal gravimetric analysis (TGA). The deprotonated ligand acts as a dibasic tridentate (ONS) via phenolate oxygen, azomethine (CN), and thiolate (C-S) groups. Copper(II) complex exhibits square planar geometry. Nickel(II), chromium(III) and dioxouranium(VI) complexes exhibit octahedral geometry. Cobalt(II), cadmium(II) and zinc(II) complexes showed tetrahedral geometry, whereas oxovanadium(IV) reveals square pyramidal geometry. Thermal analysis are investigated and showed either three or four thermal decomposition steps. Kinetic parameters (Ea, A, ΔH, ΔS and ΔG) of the thermal decomposition stages have been evaluated using Coats-Redfern equations. The molecular parameters of the ligand and its metal complexes have been calculated and correlated with the experimental data such as IR and TGA results.

  6. Crystal structure of 3-{1-[(1-allyl-1H-indazol-6-ylamino]ethylidene}-6-methyl-2H-pyran-2,4(3H-dione

    Directory of Open Access Journals (Sweden)

    Mohamed El Ghozlani

    2014-12-01

    Full Text Available In the title compound, C18H17N3O3, the dihedral angle between the planes of the indazole ring system [maximum deviation = 0.012 (1 Å] and the pyran-2,4-dione ring is 54.03 (6°. An intramolecular N—H...O hydrogen bond closes an S(6 ring. The same H atom also participates in an intermolecular N—H...O hydrogen bond, which generates an inversion dimer. The dimers are linked by weak C—H...O contacts, thereby forming a three-dimensional network.

  7. Entecavir interacts with influx transporters hOAT1, hCNT2, hCNT3, but not with hOCT2: the potential for renal transporter-mediated cytotoxicity and drug-drug interactions

    Directory of Open Access Journals (Sweden)

    František eTrejtnar

    2016-01-01

    Full Text Available Entecavir (ETV is one of the most potent agents for the treatment of the hepatitis B viral infection. The drug is principally eliminated by the kidney. The goal of this study was to investigate the potential of ETV to interact in vitro with the renal SLC transporters hOAT1, hOCT2, hCNT2 and hCNT3. Potential drug-drug interactions of ETV at the renal transporters with antiviral drugs known to be excreted by the kidney (adefovir, tenofovir, cidofovir as well as transporter-dependent cytotoxicity were also examined. Interactions with the selected transporters along with cytotoxicity were studied in several transiently-transfected cellular models using specific substrates and inhibitors. ETV was found to be both a substrate and inhibitor of hOAT1 (IC50 = 175.3 µM, hCNT2 (IC50 = 241.9 µM and hCNT3 (IC50 = 278.4 µM transporters, although it interacted with the transporters with relatively low affinities. ETV inhibited the cellular uptake of adefovir, tenofovir and cidofovir by hOAT1; however, effective inhibition was shown at ETV concentrations exceeding therapeutic levels. In comparison with adefovir, tenofovir and cidofovir, ETV displayed no transporter-mediated cytotoxicity in cells transfected with hOAT1, hCNT2, and hCNT3. No significant interaction of ETV with hOCT2 was detected. The study demonstrates interactions of ETV with several human renal transporters. For the first time, an interaction of ETV with the hCNTs was proved. We show that the potency of ETV to cause nephrotoxicity and/or clinically significant drug-drug interactions related to the tested transporters is considerably lower than that of adefovir, tenofovir and cidofovir.

  8. Spectral (FT-IR, FT-Raman, UV, and fluorescence), DFT, and solid state interaction analyses of (E)-4-(3,4-dimethoxybenzylideneamino)-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one

    Science.gov (United States)

    Alam, Mohammad Sayed; Lee, Dong-Ung

    2017-01-01

    Here, the authors report a combined experimental and theoretical study on the molecular structure and vibrational spectral analyses of (E)-4-(3,4-dimethoxybenzylideneamino)-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H)-one (DMBADPP), a pyrazolone-based bioactive molecule. Density functional theory (DFT) calculations were carried out to obtain the ground state optimized geometry of the molecule using the B3LYP method and the 6-311G(d,p) basis set. Calculated results agreed well with X-ray data. The vibrational spectra of DMBADPP were calculated at the same level of theory and theoretical scaled vibrational frequencies and assignments were found to agree well with experimental FT-IR and FT-Raman values. Partial atomic charge and molecular electrostatic potential (MEP) surface map analyses were performed to study reactive sites. Calculated frontier molecular orbitals (FMOs) energies and chemical reactivity parameters indicated that the DMBADPP exhibits high polarizability and low kinetic susceptibility. Excitation energy, wavelength, and oscillator strength were calculated using the Time Dependant-DFT/B3LYP/6-311G(d,p) method and compared with experimental UV-Vis spectra obtained in ethanol. However, UV-Vis and fluorescence spectroscopic experiments showed that DMBADPP has good absorption and fluorescent properties and a large Stokes shift. In addition, the solid state behaviors of molecules in crystals were analyzed quantitatively and qualitatively using 3D Hirshfeld surface analysis and associated 2D fingerprint plots.

  9. Synthesis and crystal structure of a copper complex with (E)-2-(4-(1H-1,2,4-triazol-1-yl)benzylidene)-3, 4-dihydronaphthalen-1(2H)-one ligand

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Shu-Wen, E-mail: sunsw0819@163.com [Yuncheng University, Department of Applied Chemistry (China); Zhang, Xiao, E-mail: zhangx@hit.edu.cn [Harbin Institute of Technology, Academy of Fundamental and Interdisciplinary Science (China); Wang, Gao-Feng [Yuncheng University, Department of Applied Chemistry (China)

    2015-12-15

    The title compound, C{sub 35}H{sub 23}CuF{sub 6}N{sub 3}O{sub 5}S{sub 2} (1), was synthesized by the reaction of Cu(tta){sub 2} and L{sup 1}, (L{sup 1} = (E)-2-(4-(1H-1,2,4-triazol-1-yl)benzylidene)-3, 4-dihydronaphthalen-1(2H)-one) in the dichloromethane solution. It crystallizes in the monoclinic, space group P2{sub 1}/c with a = 33.8388(5), b = 9.3874(2), c = 21.8194(4) Å, β = 95.522(2), V = 6898.9(2) Å{sup 3}, Z = 8, D{sub x} = 1.554 Mg/m{sup 3}, F(000) = 3272, µ = 0.834 mm{sup –1}, R{sub 1} = 0.0639, wR{sub 2} = 0.1637. The copper(II) ion of 1 is in a distorted square-pyramidal environment with four O atoms of the two tta ligands and one N atom of triazole ligand L{sup 1}. Single-crystal X-ray diffraction data revealed that the hydrogen bonds, weak C–H···π and π···π interactions in the crystals link the coordination units to form 3D supramolecular structures.

  10. Synthesis and Crystal Structure of α-(-(1,2,4-Triazol-1H-yl)-ρ-chloro Acetophenone, [ClC6H4COCH2(C2H2N3)

    Institute of Scientific and Technical Information of China (English)

    建方方; 李艳; 肖海玲; 孙萍萍

    2003-01-01

    The title compound [ClC6H4COCH2(C2H2N3)] has been prepared and characterized by elemental analysis, IR spectrum and X-ray studies. It crystallizes in the monoclinic system, space group P21/c with Mr = 221.64 (C10H8ClN3O), a = 13.420(3), b = 9.720(2), c = 7.900(2)(A°),β= 92.00(3)o, V = 1029.9(4)(A°)3, Z = 4, Dc = 1.429 g/cm3, F(000) = 456,μ = 0.345 mm-1, R = 0.0435 and wR=0.0894. The total reflections were 1949 and the independent ones were 1805 (Rint=0.0340), of which 800 were observed with I > 2σ(I). The crystal structure consists of α-(1,2,4-triazol-1H- yl)-(-chloro-acetophenone. The existence of π conjugated systems in the molecule affects partly the bond lengths. The triazole and phenyl rings form the dihedral angle of 77.34o. The molecules of the title compound connect to each other through extensive hydrogen bonds to form a two-dimensional structure. Elemental analysis and IR spectra are in good agreement with the structure data.

  11. Synthesis and crystal structure of a copper complex with ( E)-2-(4-(1 H-1,2,4-triazol-1-yl)benzylidene)-3,4-dihydronaphthalen-1(2 H)-one ligand

    Science.gov (United States)

    Sun, Shu-Wen; Zhang, Xiao; Wang, Gao-Feng

    2015-12-01

    The title compound, C35H23CuF6N3O5S2 ( 1), was synthesized by the reaction of Cu( tta)2 and L 1, ( L 1 = ( E)-2-(4-(1 H-1,2,4-triazol-1-yl)benzylidene)-3,4-dihydronaphthalen-1(2 H)-one) in the dichloromethane solution. It crystallizes in the monoclinic, space group P21/ c with a = 33.8388(5), b = 9.3874(2), c = 21.8194(4) Å, β = 95.522(2), V = 6898.9(2) Å3, Z = 8, D x = 1.554 Mg/m3, F(000) = 3272, µ = 0.834 mm-1, R 1 = 0.0639, wR 2 = 0.1637. The copper(II) ion of 1 is in a distorted square-pyramidal environment with four O atoms of the two tta ligands and one N atom of triazole ligand L 1. Single-crystal X-ray diffraction data revealed that the hydrogen bonds, weak C-H···π and π···π interactions in the crystals link the coordination units to form 3D supramolecular structures.

  12. Human PIV-2 recombinant Sendai virus (rSeV) elicits durable immunity and combines with two additional rSeVs to protect against hPIV-1, hPIV-2, hPIV-3, and RSV.

    Science.gov (United States)

    Jones, Bart; Zhan, Xiaoyan; Mishin, Vasiliy; Slobod, Karen S; Surman, Sherri; Russell, Charles J; Portner, Allen; Hurwitz, Julia L

    2009-03-13

    The human parainfluenza viruses (hPIVs) and respiratory syncytial viruses (RSVs) are the leading causes of hospitalizations due to respiratory viral disease in infants and young children, but no vaccines are yet available. Here we describe the use of recombinant Sendai viruses (rSeVs) as candidate vaccine vectors for these respiratory viruses in a cotton rat model. Two new Sendai virus (SeV)-based hPIV-2 vaccine constructs were generated by inserting the fusion (F) gene or the hemagglutinin-neuraminidase (HN) gene from hPIV-2 into the rSeV genome. The inoculation of either vaccine into cotton rats elicited neutralizing antibodies toward both homologous and heterologous hPIV-2 virus isolates. The vaccines elicited robust and durable antibodies toward hPIV-2, and cotton rats immunized with individual or mixed vaccines were fully protected against hPIV-2 infections of the lower respiratory tract. The immune responses toward a single inoculation with rSeV vaccines were long-lasting and cotton rats were protected against viral challenge for as long as 11 months after vaccination. One inoculation with a mixture of the hPIV-2-HN-expressing construct and two additional rSeVs (expressing the F protein of RSV and the HN protein of hPIV-3) resulted in protection against challenge viruses hPIV-1, hPIV-2, hPIV-3, and RSV. Results identify SeV vectors as promising vaccine candidates for four different paramyxoviruses, each responsible for serious respiratory infections in children.

  13. Novel Isatin-Schiff Base Cu (H) and Ni(H) Complexes. X-ray Crystal Structure of Bis[3-(4-hexylphenylimino)-1H-indol-2(3H)-one]-dichlorocopper(H) Complex

    Institute of Scientific and Technical Information of China (English)

    Ayse ERCAG; Sema Oztürk YILDIRIM; Mehmet AKKURT; Mahmure Ustün OZGUR; Frank W. HEINEMANN

    2006-01-01

    Schiff base ligand (HL) derived from 4-hexylaniline with isatin (1H-indole-2,3-dione)and its complexes with Cu(Ⅱ), Ni(Ⅱ) were prepared and characterized by analytical, spectroscopic (IR, UV-Vis, Mass) techniques, electrical conductivity, magnetic and thermal measurements. The crystal and molecular structure of [Cu(HL)2Cl2] was determined by a single-crystal X-ray diffraction study. The molecular structure of the title compound has an inversion center on the Cu atom.

  14. Synthesis of pyrrolo[2,1-f][1,2,4]triazin-4(3H-ones: Rearrangement of pyrrolo[1,2-d][1,3,4]oxadiazines and regioselective intramolecular cyclization of 1,2-biscarbamoyl-substituted 1H-pyrroles

    Directory of Open Access Journals (Sweden)

    Kkonnip Son

    2016-08-01

    Full Text Available Pyrrolo[2,1-f][1,2,4]triazin-4(3H-ones 12 have been easily prepared via nucleophile-induced rearrangement of pyrrolooxadiazines 11 and regioselective intramolecular cyclization of 1,2-biscarbamoyl-substituted 1H-pyrroles 10. In this work, we demonstrated that the described synthetic approaches can be considered to be more facile and practical than previously reported procedures.

  15. An efficient synthesis of novel 3’-substituted 2-aryl-5-methyl-5'thioxo-[4,4'-bi-4H-1,2,4-triazol]-3(1'H, 2H-ones

    Directory of Open Access Journals (Sweden)

    RAVINDRA R. KAMBLE

    2006-04-01

    Full Text Available Asimple and high yieldingmethod for the integration of two 1,2,4-triazole rings (10a–l has been developed starting from 3-arylsydnones (1a–d. Confirmation for the structures of the newly synthesised compounds was provided by their physical, analytical and spectral data (IR, 1H NMR, 13C NMR and MS.

  16. Copper diphosphonates with zero-, one- and two-dimensional structures: ferrimagnetism in layer compound Cu3(ImhedpH)(2).2H2O [ImhedpH4=(1-C3H3N2)CH2C(OH)(PO3H2)2].

    Science.gov (United States)

    Cao, Deng-Ke; Xie, Xiao-Ji; Li, Yi-Zhi; Zheng, Li-Min

    2008-10-07

    Reactions of CuSO4 with 2-(1-imidazole)-1-hydroxy-1,1'-ethylidenediphosphonic acid (ImhedpH4) under hydrothermal conditions at different temperatures lead to four new metal phosphonates: Cu(ImhedpH3)2(H2O).2H2O (), Cu(ImhedpH3)2 (), Cu3(ImhedpH2)2(ImhedpH3)(2).4H2O (), and Cu3(ImhedpH)(2).2H2O (). Compounds and have mononuclear structures in which the Cu atoms adopt square pyramidal and square planar geometries, respectively. In compound , a chain structure is observed where the Cu3(ImhedpH2)2(ImhedpH3)2 trimer units are connected by edge-sharing of the {Cu2O5} square pyramids. Compound exhibits a layer structure made up of Cu3(ImhedpH)2 trimer units. The connection of trimers through corner-sharing of {Cu1O4} and {CPO3} tetrahedra results in a two-dimensional layer containing 8- and 16-membered rings. The imidazole groups are grafted on the two sides of the layer. Magnetic studies reveal that ferromagnetic interactions are mediated in , while for compound , ferrimagnetism is observed below 5.8 K.

  17. A novel and potent poly(ADP-ribose) polymerase-1 inhibitor, FR247304 (5-chloro-2-[3-(4-phenyl-3,6-dihydro-1(2H)-pyridinyl)propyl]-4(3H)-quinazolinone), attenuates neuronal damage in in vitro and in vivo models of cerebral ischemia.

    Science.gov (United States)

    Iwashita, Akinori; Tojo, Nobuteru; Matsuura, Shigeru; Yamazaki, Syunji; Kamijo, Kazunori; Ishida, Junya; Yamamoto, Hirofumi; Hattori, Kouji; Matsuoka, Nobuya; Mutoh, Seitaro

    2004-08-01

    The activation of poly(ADP-ribose) polymerase-1 (PARP-1) after exposure to nitric oxide or oxygen-free radicals can lead to cell injury via severe, irreversible depletion of NAD. Genetic deletion or pharmacological inhibition of PARP-1 attenuates brain injury after focal ischemia and neurotoxicity in several neurodegenerative models in animals. FR247304 (5-chloro-2-[3-(4-phenyl-3,6-dihydro-1(2H)-pyridinyl)propyl]-4(3H)-quinazolinone) is a novel PARP-1 inhibitor that has recently been identified through structure-based drug design. In an enzyme kinetic analysis, FR247304 exhibits potent and competitive inhibition of PARP-1 activity, with a K(i) value of 35 nM. Here, we show that prevention of PARP activation by FR247304 treatment protects against both reactive oxygen species-induced PC12 cell injury in vitro and ischemic brain injury in vivo. In cell death model, treatment with FR247304 (10(-8)-10(-5) M) significantly reduced NAD depletion by PARP-1 inhibition and attenuated cell death after hydrogen peroxide (100 microM) exposure. After 90 min of middle cerebral artery occlusion in rats, poly(ADP-ribosy)lation and NAD depletion were markedly increased in the cortex and striatum from 1 h after reperfusion. The increased poly(ADP-ribose) immunoreactivity and NAD depletion were attenuated by FR247304 (32 mg/kg i.p.) treatment, and FR247304 significantly decreased ischemic brain damage measured at 24 h after reperfusion. Whereas other PARP inhibitors such as 3-aminobenzamide and PJ34 [N-(6-oxo-5,6-dihydro-phenanthridin-2-yl)-N,N-dimethylactamide] showed similar neuroprotective actions, they were less potent in in vitro assays and less efficacious in an in vivo model compared with FR247304. These results indicate that the novel PARP-1 inhibitor FR247304 exerts its neuroprotective efficacy in in vitro and in vivo experimental models of cerebral ischemia via potent PARP-1 inhibition and also suggest that FR247304 or its derivatives could be attractive therapeutic

  18. Determination of the 2H/1H and 15N/14N ratios of Alkylpyrazines from coffee beans (Coffea arabica L. and Coffea canephoravar. robusta) by isotope ratio mass spectrometry.

    Science.gov (United States)

    Richling, Elke; Preston, Christina; Kavvadias, Dominique; Kahle, Kathrin; Heppel, Christopher; Hummel, Silvia; König, Thorsten; Schreier, Peter

    2005-10-05

    The delta15N(AIR) and delta2H(VSMOW) data for several alkylpyrazines formed during the roasting process of coffee are reported. Samples of commercially available roasted (n = 9) as well as self-roasted (n = 8) coffee beans (Coffea arabica L. and Coffea canephora var. robusta) of different origins were investigated. By use of extracts prepared by simultaneous distillation extraction (SDE) and subsequently fractionated by liquid chromatography on silica gel, on-line capillary gas chromatography-isotope ratio mass spectrometry was employed in the combustion (C) and pyrolysis (P) modes (HRGC-C/P-IRMS) to determine the delta15N(AIR) and delta2H(VSMOW) values, respectively. In addition to the constituents of coffee beans, data for commercial synthetic alkylpyrazines and substances declared to be "natural" were determined. The delta15N(AIR) data for coffee alkylpyrazines under study-2-ethyl-5-methylpyrazine (1) and 2-ethyl-6-methylpyrazine (2) (measured as sum 1/2), 2-ethyl-3-methylpyrazine (3), 2-methylpyrazine (4), 2,5-dimethylpyrazine (5) and 2,6-dimethylpyrazine (6) (measured as sum 5/6), and 2,3-dimethylpyrazine (7), as well as 2,3,5-trimethylpyrazine (8)-varied in the range from +8.3 to -10.2 per thousand, thus revealing their biogeneration from amino acids (delta15N(AIR) ranging from +8 per thousand to -10 per thousand). The delta2H(VSMOW) values were determined in the range from -5 per thousand to -127 per thousand. Owing to the analytical differentiation observed between coffee alkylpyrazines and synthetic/"natural" samples of 3, 4, and 7, authenticity assessment of coffee-flavored products seems to be promising, provided that extended data will be available in the future. In the literature, there were no IRMS data available for the alkylpyrazines (1-8) under study.

  19. Ion-neutral reactions in the ion source of a mixture of CO2/CH3OH, CO2/C2H5OH, and CO2/2-C3H7OH by packed capillary supercritical fluid chromatography-mass spectrometry (SFC-MS).

    Science.gov (United States)

    Ekeberg, Dag; Jablonska-Jentoft, Anja M

    2007-12-01

    Ion neutral reactions in the gas phase in mixtures of ROH/CO(2), R = CH(3), C(2)H(5), and 2-C(3)H(7) were studied by supercritical fluid chromatography-mass spectrometry (SFC-MS). Three main reaction series were found for this system; ionization followed by alpha-cleavage, formation of clusters, and formation of protonated dialkyl ethers from the corresponding alcohol. The ion chemistries were similar for the three alcohols, but that of 2-propanol was somewhat more complex.

  20. [[sup 3]H]imidacloprid: synthesis of a candidate radioligand for the nicotinic acetylcholine receptor

    Energy Technology Data Exchange (ETDEWEB)

    Latli, B.; Casida, J.E. (California Univ., Berkeley, CA (United States). Dept. of Entomological Sciences)

    1992-08-01

    Imidacloprid is an exceptionally potent insecticide known from physiological studies to act at the nicotinic acetylcholine receptor. To prepare [[sup 3]H]imidacloprid as a candidate radioligand, 6-chloronicotinoyl chloride was reduced with NaB[sup 2]H[sub 4] (in model studies) or NaB[sup 3]H[sub 4] in absolute ethanol to 2-chloro-5-pyridinylmethanol which was transformed to 2-chloro-5-chloromethylpyridine on refluxing with thionyl chloride. Coupling with 4,5-dihydro-N-nitro-1H-imidazol-2-amine then gave [[sup 2]H[sub 2

  1. In Silico Identification of Highly Conserved Epitopes of Influenza A H1N1, H2N2, H3N2, and H5N1 with Diagnostic and Vaccination Potential

    Directory of Open Access Journals (Sweden)

    José Esteban Muñoz-Medina

    2015-01-01

    Full Text Available The unpredictable, evolutionary nature of the influenza A virus (IAV is the primary problem when generating a vaccine and when designing diagnostic strategies; thus, it is necessary to determine the constant regions in viral proteins. In this study, we completed an in silico analysis of the reported epitopes of the 4 IAV proteins that are antigenically most significant (HA, NA, NP, and M2 in the 3 strains with the greatest world circulation in the last century (H1N1, H2N2, and H3N2 and in one of the main aviary subtypes responsible for zoonosis (H5N1. For this purpose, the HMMER program was used to align 3,016 epitopes reported in the Immune Epitope Database and Analysis Resource (IEDB and distributed in 34,294 stored sequences in the Pfam database. Eighteen epitopes were identified: 8 in HA, 5 in NA, 3 in NP, and 2 in M2. These epitopes have remained constant since they were first identified (~91 years and are present in strains that have circulated on 5 continents. These sites could be targets for vaccination design strategies based on epitopes and/or as markers in the implementation of diagnostic techniques.

  2. ON THE FORMATION AND ISOMER SPECIFIC DETECTION OF PROPENAL (C{sub 2}H{sub 3}CHO) AND CYCLOPROPANONE (c-C{sub 3}H{sub 4}O) IN INTERSTELLAR MODEL ICES—A COMBINED FTIR AND REFLECTRON TIME-OF-FLIGHT MASS SPECTROSCOPIC STUDY

    Energy Technology Data Exchange (ETDEWEB)

    Abplanalp, Matthew J.; Borsuk, Aleca; Jones, Brant M.; Kaiser, Ralf I., E-mail: ralfk@hawaii.edu [W. M. Keck Research Laboratory in Astrochemistry, University of Hawaii at Manoa, Honolulu, Hawaii, HI, 96822 (United States)

    2015-11-20

    The formation routes of two structural isomers—propenal (C{sub 2}H{sub 3}CHO) and cyclopropanone (c-C{sub 3}H{sub 4}O)—were investigated experimentally by exposing ices of astrophysical interest to energetic electrons at 5.5 K thus mimicking the interaction of ionizing radiation with interstellar ices in cold molecular clouds. The radiation-induced processing of these ices was monitored online and in situ via Fourier Transform Infrared spectroscopy and via temperature programmed desorption exploiting highly sensitive reflectron time-of-flight mass spectrometry coupled with single photon ionization in the post irradiation phase. To selectively probe which isomer(s) is/are formed, the photoionization experiments were conducted with 10.49 and 9.60 eV photons. Our studies provided compelling evidence on the formation of both isomers—propenal (C{sub 2}H{sub 3}CHO) and cyclopropanone (c-C{sub 3}H{sub 4}O)—in ethylene (C{sub 2}H{sub 4})—carbon monoxide (CO) ices forming propenal and cyclopropanone at a ratio of (4.5 ± 0.9):1. Based on the extracted reaction pathways, the cyclopropanone molecule can be classified as a tracer of a low temperature non-equilibrium chemistry within interstellar ices involving most likely excited triplet states, whereas propenal can be formed at ultralow temperatures, but also during the annealing phase via non-equilibrium as well as thermal chemistry (radical recombination). Since propenal has been detected in the interstellar medium and our laboratory experiments demonstrate that both isomers originated from identical precursor molecules our study predicts that the hitherto elusive second isomer—cyclopropanone—should also be observable toward those astronomical sources such as Sgr B2(N) in which propenal has been detected.

  3. CAF-1-induced oligomerization of histones H3/H4 and mutually exclusive interactions with Asf1 guide H3/H4 transitions among histone chaperones and DNA.

    Science.gov (United States)

    Liu, Wallace H; Roemer, Sarah C; Port, Alex M; Churchill, Mair E A

    2012-12-01

    Anti-silencing function 1 (Asf1) and Chromatin Assembly Factor 1 (CAF-1) chaperone histones H3/H4 during the assembly of nucleosomes on newly replicated DNA. To understand the mechanism of histone H3/H4 transfer among Asf1, CAF-1 and DNA from a thermodynamic perspective, we developed and employed biophysical approaches using full-length proteins in the budding yeast system. We find that the C-terminal tail of Asf1 enhances the interaction of Asf1 with CAF-1. Surprisingly, although H3/H4 also enhances the interaction of Asf1 with the CAF-1 subunit Cac2, H3/H4 forms a tight complex with CAF-1 exclusive of Asf1, with an affinity weaker than Asf1-H3/H4 or H3/H4-DNA interactions. Unlike Asf1, monomeric CAF-1 binds to multiple H3/H4 dimers, which ultimately promotes the formation of (H3/H4)(2) tetramers on DNA. Thus, transition of H3/H4 from the Asf1-associated dimer to the DNA-associated tetramer is promoted by CAF-1-induced H3/H4 oligomerization.

  4. Antitumor activity of 6-(cyclohexylamino)-1, 3-dimethyl-5(2-pyridyl)furo[2,3-d]pyrimidine-2,4(1H,3H)-dione and Its Ti(IV), Zn(II), Fe(III), and Pd(II) complexes on K562 and Jurkat cell lines.

    Science.gov (United States)

    Shabani, Fahmideh; Ghammamy, Shahriar; Mehrani, Khayroallah; Teimouri, Mohammad Bagher; Soleimani, Masoud; Kaviani, Saeid

    2008-01-01

    (6-(cyclohexylamino)-1,3-dimethyl-5(2-pyridyl)furo[2,3-d]pyrimidine-2,4(1H,3H)-dione) abbreviated as CDP was synthesized and characterized. Ti(IV), Zn(II), Fe(III), and Pd(II) metal complexes of this ligand are prepared by the reaction of salts of Ti(IV), Zn(II), Fe(III), and Pd(II) with CDP in acetonitrile. Characterization of the ligand and its complexes was made by microanalyses, FT-IR, (1)H NMR, (13)C NMR, and UV-Visible spectroscopy. All complexes were characterized by several techniques using elemental analysis (C, H, N), FT-IR, electronic spectra, and molar conductance measurements. The elemental analysis data suggest the stoichiometry to be 1:1 [M:L] ratio formation. The molar conductance measurements reveal the presence of 1:1 electrolytic nature complexes. These new complexes showed excellent antitumor activity against two kinds of cancer cells that are K562 (human chronic myeloid leukemia) cells and Jurkat (human T lymphocyte carcinoma) cells.

  5. Electronic structures and selective fluoride sensing features of Os(bpy)2(HL(2-)) and [{Os(bpy)2}2(μ-HL(2-))](2+) (H3L: 5-(1H-benzo[d]imidazol-2-yl)-1H-imidazole-4-carboxylic acid).

    Science.gov (United States)

    Das, Ankita; Agarwala, Hemlata; Kundu, Tanaya; Ghosh, Prabir; Mondal, Sudipta; Mobin, Shaikh M; Lahiri, Goutam Kumar

    2014-10-07

    The article deals with the newly designed mononuclear and asymmetric dinuclear osmium(ii) complexes Os(II)(bpy)2(HL(2-)) (1) and [(bpy)2Os(II)(μ-HL(2-))Os(II)(bpy)2](Cl)2 ([2](Cl)2)/[(bpy)2Os(II)(μ-HL(2-))Os(II)(bpy)2](ClO4)2 ([2](ClO4)2), respectively, (H3L = 5-(1H-benzo[d]imidazol-2-yl)-1H-imidazole-4-carboxylic acid and bpy = 2,2'-bipyridine). The identity of 1 has been established by its single crystal X-ray structure. The ligand (HL(2-))-based primary oxidation process (E, 0.23 V versus SCE) along with the partial metal contribution (∼20%) in 1 has been revealed by the ligand-dominated HOMO of 1 (HL(2-): 88%, Os: 8%), as well as by the Mulliken spin density distribution of 1(+) (HL(2-): 0.878, Os: 0.220). Accordingly, 1(+) exhibits a free radical type EPR at 77 K with a partial metal-based anisotropic feature (g1 = 2.127, g2 = 2.096, g3 = 2.046; = 2.089; Δg = 0.08). (1)H-NMR of the dinuclear 2(2+) in CDCl3 suggests an intimate mixture of two diastereomeric forms in a 1 : 1 ratio. The DFT-supported predominantly Os(ii)/Os(iii)-based couples of asymmetric 2(2+) at 0.24 V and 0.50 V versus SCE result in a comproportionation constant (Kc) value of 8.2 × 10(4). The class I mixed valent state of 2(3+) (S = 1/2) has, however, been corroborated by the Mulliken spin density distribution of Os1: 0.887, Os2: 0.005, HL(2-): 0.117, as well as by the absence of a low-energy IVCT (intervalence charge transfer) band in the near-IR region (up to 2000 nm). The appreciable spin accumulation on the bridge in 2(3+) or 2(4+) (S = 1, Os1: 0.915, Os2: 0.811 and HL(2-): 0.275) implies a mixed electronic structural form of [(bpy)2Os(III)(μ-HL(2-))Os(II)(bpy)2](3+)(major)/[(bpy)2Os(II)(μ-HL˙(-))Os(II)(bpy)2](3+)(minor) or [(bpy)2Os(III)(μ-HL(2-))Os(III)(bpy)2](4+)(major)/[(bpy)2Os(III)(μ-HL˙(-))Os(II)(bpy)2](4+) (minor), respectively. The mixed valent {Os(III)(μ-HL(2-))Os(II)} state in 2(3+), however, fails to show EPR at 77 K due to the rapid spin relaxation process

  6. Metal-ligand interaction of lanthanides with coumarin derivatives. Part I. Complexation of 3-(1-aminoethylidene)-2H-chromene-2,4(3H)-dione with La(III), Ce(III), Nd(III) and Ho(III).

    Science.gov (United States)

    Swiatek, Mirosława; Kufelnicki, Aleksander

    2012-01-01

    Solutions of lanthanum(III), cerium(III), neodymium(III) and holmium(III) nitrates with 3-(1-aminoethylidene)-2H-chromene-2,4(3H)-dione (1) in 10% v/v dioxane-water medium were used. Coordination modes of 1 with the selected lanthanides have been examined. Hydroxo-complexes with deprotonated water molecules from the inner coordination sphere have been stated in basic medium. Stability constants of the forming complex species were determined by potentiometric titrations using Superquad and Hyperquad2003 programs. The most stable complexes are formed with La(III). The UV-Vis spectra of the Nd(III)-1 system confirmed the L:M = 1:1 stoichiometry evaluated potentiometrically.

  7. Studies of the mechanism of the olefin metathesis reaction and the process of active site formation on photoreduced molybdenum-silicate catalysts. 2. Productive and degenerative metathesis of C/sub 2/H/sub 4/-C/sub 2/D/sub 4/ and C/sub 3/H/sub 6/-C/sub 3/D/sub 6/ mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Elev, I.V.; Shelimov, B.N.; Kazanskii, V.B.

    1987-10-01

    The specific catalytic activity of photoreduced Mo/sup 4 +//SiO/sub 2/ samples has been compared for productive and degenerate metathesis reactions of C/sub 3/H/sub 6/-C/sub 3/D/sub 6/ and C/sub 2/H/sub 4/-C/sub 2/D/sub 4/ mixtures. It has been found, that, under comparable conditions, the rate of degenerate metathesis of ethylene is 4-5 times slower than the rate of productive metathesis of propylene, although the rate of degenerate metathesis of propylene is 5 x 10/sup 3/-10/sup 4/ times greater than its rate of productive metathesis. Based on these results, it is concluded that degenerate metathesis of propylene occurs via the involvement of secondary (ethylidene) carbenes.

  8. Ligand and substrate effects in gas-phase reactions of NiX(+)/RH couples (X=F, Cl, Br, I; R=CH3, C2H5, nC3H7, nC4H9).

    Science.gov (United States)

    Schlangen, Maria; Schröder, Detlef; Schwarz, Helmut

    2007-01-01

    The reactions of small saturated hydrocarbons by gaseous nickel cations NiX+ (X=F, Cl, Br, I) are investigated by means of electrospray ionization mass spectrometry. The halide cations are obtained from solutions of the corresponding Ni(II) salts in water or methanol as solvents. NiF+ is the only Ni(II) halide complex that brings about thermal activation of methane. The branching ratios of the observed reactions with C2H6, C3H8, and nC4H10 are shifted systematically by changing the nature of both the ligand X and the substrate RH. In the elimination of HX (X=F, Cl, Br, I), the formal oxidation state of the metal ion appears to be conserved, and the importance of this reaction channel decreases in going from NiF+ to NiI+. A reversed trend is observed in the losses of small closed-shell neutral molecules, that is, H2, CH4 and C2H6, which dominate the gas-phase ion chemistry of NiI+/RH couples. Additionally, inner-sphere electron-transfer reactions take place for a few systems, that is, the delivery of hydride or methanide ions from the hydrocarbon to NiX+ in the course of which the hydrocarbon is converted to a carbenium ion and the cationic metal complex gives rise to a neutral RNiX molecule (R=H, CH3). This process gains importance with decreasing atomic number of the halides and with increasing the size of the alkane. Thus, it constitutes the major pathway in the reactions of NiF+ with propane and n-butane, whereas it is not observed for any of the NiI+/RH couples investigated. Concerning the regioselectivity of the reactions with propane and n-butane, heterolytic cleavage of secondary carbon--hydrogen bonds is clearly preferred compared to that of primary ones, as revealed by deuterium labeling studies. For the NiF+/C3H8 couple, the selectivity of the hydride transfer is as large as 360 in favor of the secondary positions. Though smaller, large preferences for the activation of secondary C--H bonds are also operative in homolytic bond activation of RH (R=nC3H7, n

  9. Crystal structure of new uranyl oxalates (NH{sub 4}){sub 2}[UO{sub 2}(C{sub 2}O{sub 4}){sub 2}.H{sub 2}O].2H{sub 2}O and (NH{sub 4}){sub 2-x}(N{sub 2}H{sub 5}){sub x}[(UO{sub 2}){sub 2}(C{sub 2}O{sub 4}){sub 3}].3H{sub 2}O (x = 0 and x = 1). Comparison with other uranyl oxalates

    Energy Technology Data Exchange (ETDEWEB)

    Chapelet-Arab, B. [Lab. de Cristallochimie et Physicochimie du Solide, UMR CNRS, Villeneuve d' Ascq (France); Lab. de Chimie des Actinides, CEA VALRHO/DRCP/SCPS, Bagnols sur Ceze (France); Nowogrocki, G.; Abraham, F. [Lab. de Cristallochimie et Physicochimie du Solide, UMR CNRS, Villeneuve d' Ascq (France); Grandjean, S. [Lab. de Chimie des Actinides, CEA VALRHO/DRCP/SCPS, Bagnols sur Ceze (France)

    2005-07-01

    Two new ammonium uranyl oxalates (NH{sub 4}){sub 2}[UO{sub 2}(C{sub 2}O{sub 4}){sub 2}H{sub 2}O].2H{sub 2}O (1) and (NH{sub 4}){sub 2}[(UO{sub 2}){sub 2}(C{sub 2}O{sub 4}){sub 3}].3H{sub 2}O (2) and one mixed ammonium hydrazinium uranyl oxalate (NH{sub 4})(N{sub 2}H{sub 5})[(UO{sub 2}){sub 2}(C{sub 2}O{sub 4}){sub 3}].3H{sub 2}O (3) have been prepared. The crystal structures of the three compounds have been determined by single-crystal X-ray diffraction. The crystal structures were solved by the Patterson method and Fourier difference techniques, and refined by a least square method on the basis of F{sup 2} for all unique reflections. Crystallographic data: 1, hexagonal, space group P6{sub 1}22, a = 8.143(2) Aa, c = 36.179(18) Aa, Z = 6, R1 = 0.0268 for 105 parameters with 1223 reflections with I {>=} 2{sigma}(I); 2, monoclinic, space group P2{sub 1}/n, a = 8.705(3) Aa, b = 19.454(6) Aa, c = 5.5105(18) Aa, {beta} = 101.741(5) , Z = 2, R1 = 0.0314 for 139 parameters with 2059 reflections with I {>=} 2{sigma}(I); 3, monoclinic, space group P2{sub 1}/n, a = 8.958(3) Aa, b = 19.601(7) Aa, c = 11.007(4) Aa, {beta} = 112.928(5) , Z = 4, R1 = 0.0363 for 131 parameters with 3346 reflections with I {>=} 2{sigma}(I). The crystal structure of 1 contains [UO{sub 2}(C{sub 2}O{sub 4}){sub 2}.H{sub 2}O]{sup 2-} anions, NH{sub 4}{sup +} cations and water molecules. In the anion, the linear uranyl group is coordinated by two bidentate oxalate anions and one water molecule giving a pentagonal bipyramidal environment for the uranium atom. The structures of 2 and 3 consist of two-dimensional networks built from uranyl and oxalate ions forming hexagonal rings. The oxalate ions are tetradentate, each bridging two uranyl ions which are coordinated by three oxalate groups to give distorted hexagonal bipyramidal environments for the uranium atoms. In 3, the ammonium and hydrazinium ions are ordered in successive layers. The various possible coordinations for the uranyl cation and the great

  10. Synthesis, Crystal Structure and Thermal Stability of a Novel Hetero-bimetallic Complex: Bis(malonato)tetra-(aqua)calcum(Ⅱ)copper(Ⅱ)%杂-双核配合物[CaCu(C3H2O4)2(H2O)4]n的合成、晶体结构及热稳定性

    Institute of Scientific and Technical Information of China (English)

    傅绪成; 王成刚; 李明田; 王小艳

    2007-01-01

    The title complex, [CaCu(C3H2O4)2(H2O)4]n, with a formula of C6H12CaCuO12 and Mr=379.78 has been synthesized and characterized by single crystal X-ray diffraction structure analysis, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is Orthorhombic, space group Pbcn with a=0.669 21(5)and Z=4. The final R=0.0540 and wR=0.112 8 for 1 189 observed reflections with I>2σ(Ⅰ). The structure of the title complex consists of CaO8 polyhedra and CuO6 elongated octahedra linked together by malonate ligands. The Ca(Ⅱ) cation, on a twofold axis, is coordinated by two water molecules and six malonate O atoms. The Cu(Ⅱ)cation, which lies in a centre of symmetry in an octahedral arrangement, is coordinated by four malonate O atoms Cu distance of 0.762 46(6) nm. The whole 3D structure is maintained and stabilized by the presence of hydrogen bonds. Its thermo gravimetric analysis was determined by TG-DTG techniques. CCDC: 663184.

  11. Crystal structure of (E)-2-[(2-bromopyridin-3-yl)methyl-idene]-6-meth-oxy-3,4-di-hydro-naphthalen-1(2H)-one and 3-[(E)-(6-meth-oxy-1-oxo-1,2,3,4-tetra-hydro-naphthalen-2-ylidene)meth-yl]pyridin-2(1H)-one.

    Science.gov (United States)

    Zingales, Sarah K; Moore, Morgan E; Goetz, Andrew D; Padgett, Clifford W

    2016-07-01

    The title compounds C17H14BrNO2, (I), and C17H15NO3, (II), were obtained from the reaction of 6-meth-oxy-3,4-di-hydro-2H-naphthalen-1-one and 2-bromo-nicotinaldehyde in ethanol. Compound (I) was the expected product and compound (II) was the oxidation product from air exposure. In the crystal structure of compound (I), there are no short contacts or hydrogen bonds. The structure does display π-π inter-actions between adjacent benzene rings and adjacent pyridyl rings. Compound (II) contains two independent mol-ecules, A and B, in the asymmetric unit; both are non-planar, the dihedral angles between the meth-oxy-benzene and 1H-pyridin-2-one mean planes being 35.07 (9)° in A and 35.28 (9)°in B. In each mol-ecule, the 1H-pyridin-2-one unit participates in inter-molecular N-H⋯O hydrogen bonding to another mol-ecule of the same type (A to A or B to B). The structure also displays π-π inter-actions between the pyridyl and the benzene rings of non-equivalent mol-ecules (viz., A to B and B to A).

  12. Crystal structure of (E-2-[(2-bromopyridin-3-ylmethylidene]-6-methoxy-3,4-dihydronaphthalen-1(2H-one and 3-[(E-(6-methoxy-1-oxo-1,2,3,4-tetrahydronaphthalen-2-ylidenemethyl]pyridin-2(1H-one

    Directory of Open Access Journals (Sweden)

    Sarah K. Zingales

    2016-07-01

    Full Text Available The title compounds C17H14BrNO2, (I, and C17H15NO3, (II, were obtained from the reaction of 6-methoxy-3,4-dihydro-2H-naphthalen-1-one and 2-bromonicotinaldehyde in ethanol. Compound (I was the expected product and compound (II was the oxidation product from air exposure. In the crystal structure of compound (I, there are no short contacts or hydrogen bonds. The structure does display π–π interactions between adjacent benzene rings and adjacent pyridyl rings. Compound (II contains two independent molecules, A and B, in the asymmetric unit; both are non-planar, the dihedral angles between the methoxybenzene and 1H-pyridin-2-one mean planes being 35.07 (9° in A and 35.28 (9°in B. In each molecule, the 1H-pyridin-2-one unit participates in intermolecular N—H...O hydrogen bonding to another molecule of the same type (A to A or B to B. The structure also displays π–π interactions between the pyridyl and the benzene rings of non-equivalent molecules (viz., A to B and B to A.

  13. 7-Chloro-5-(4-hydroxyphenyl)-1-methyl-3-(naphthalen-2-ylmethyl)-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (Bz-423), a benzodiazepine, suppresses keratinocyte proliferation and has antipsoriatic activity in the human skin-severe, combined immunodeficient mouse transplant model.

    Science.gov (United States)

    Bhagavathula, Narasimharao; Nerusu, Kamalakar C; Hanosh, Andrew; Aslam, Muhammad N; Sundberg, Thomas B; Opipari, Anthony W; Johnson, Kent; Kang, Sewon; Glick, Gary D; Varani, James

    2008-03-01

    7-Chloro-5-(4-hydroxyphenyl)-1-methyl-3-(naphthalen-2-ylmethyl)-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (Bz-423) is a benzodiazepine that has cytotoxic and cytostatic activity against a variety of cells in vivo and in vitro. In the present study, we demonstrate that Bz-423 (formulated for topical delivery) reduces epidermal hyperplasia in human psoriatic skin after transplantation to severe, combined immunodeficient (scid) mice. Bz-423 also suppresses the hyperplasia that develops in nonpsoriatic human skin as a consequence of transplantation to scid mice. Proliferation of human epidermal keratinocytes in monolayer culture was suppressed by Bz-423 at concentrations of 0.5 to 2.0 muM (noncytotoxic concentrations). Keratinocyte growth inhibition was accompanied by increased oxidant generation in Bz-423-treated cells, and treatment with vitamin E along with Bz-423 reversed the growth inhibition. Growth inhibition was accompanied by a redistribution of beta-catenin from a cytoplasmic pool to the cell membrane and by reduced levels of c-myc and cyclin D1 (two molecules associated with Wnt pathway signaling). Several analogs of Bz-423 were examined for antiproliferative activity against human epidermal keratinocytes and human dermal fibroblasts in monolayer culture. Each of the analogs tested suppressed growth of both cell types, but in all cases, keratinocytes were more sensitive than fibroblasts. Two of the compounds were found to suppress epidermal hyperplasia induced with all-trans retinoic acid in organ cultures of human skin. Taken together, these data show that Bz-423 and certain analogs produce biological responses in skin cells in vitro and in vivo that are consistent with therapeutic goals for treating psoriasis or epidermal hyperplasia resulting from other causes.

  14. The Hydrothermal NH 4/V/P/H 2O and K/v/p/n(c 2H 5) 3/H 2O Systems at 473 K and the Crystal Structures of NH 4VOPO 4and (nh 4) 3V 2O 3(VO)(PO 4) 2(HPO 4)

    Science.gov (United States)

    Schindler, Michael; Joswig, Werner; Baur, Werner H.

    1997-12-01

    An examination of the NH 4/VO 5/P/H 2O system at 473 K under hydrothermal conditions yielded the (NH 4) 3V 2O 3(VO)(PO 4) 2(HPO 4) and NH 4VOPO 4phases. The crystal structure of the first compound is isotypical with the corresponding Tl +and K +phases. The cations NH +4and Tl +have similar coordinations against oxygen. The investigation of the crystal structure of the second compound (space group Pn2 n) shows it to be related to other ABO TO 4phases of the potassium titanyl phosphate type with A=Na +, Ag +, NH +4, Rb +, K +, and Tl +, and B=Ti 4+, V 4+, Sn 4+, Fe 4+, Ge 4+, Ga 3+, Zr 4+, Sb 5+, and Nb 5+, and T=P 5+, Ge 4+, Si 4+, and As 5+, but none of them crystallize in space group Pn2 n. In the K/V/P/N(C 2H 5) 3/H 2O system, three different K phases were found: K 0.5VOPO 4·1.5H 2O, KVOPO 4, and K-FVP-1 (Frankfurt vanadium phosphate, one, or for short, FVP-1). The microporous K-FVP-1 compound was synthesized in a similar pH range as the isotypic Na-FVP-1 phase. The V 4+/V 5+ratio of K-FVP-1 varies from 3.5(1)/1.5(1) to 1.6(1)/3.4(1) and the corresponding lattice constants range from 16.0013(6) to 15.7665(4) Å.

  15. (3aS,7aS-5-[(S-3,3,3-Trifluoro-2-methoxy-2-phenylpropanoyl]-2,3,4,5,6,7-hexahydro-1H-pyrrolo[3,4-c]pyridin-3(2H-one monohydrate

    Directory of Open Access Journals (Sweden)

    Huichun Zhu

    2010-01-01

    Full Text Available rac-Benzyl 3-oxohexahydro-1H-pyrrolo[3,4-c]pyridine-5(6H-carboxylate was separated by chiral chromatography, and one of the enantiomers ([α]22D = +10° was hydrogenated in the presence of Pd/C in methanol, producing octahydro-3H-pyrrolo[3,4-c]pyridin-3-one. The latter was reacted with (2R-3,3,3-trifluoro-2-methoxy-2-phenylpropanoyl chloride [(R-(−-Mosher acid chloride], giving rise to the title compound, C17H19F3N2O3·H2O. The present structure established the absolute configuration of the pyrrolopiperidine fragment based on the known configuration of the (R-Mosher acid chloride. The piperidine ring has a somewhat distorted chair conformation and is cis-fused with the five-membered envelope-shaped ring; the plane of the exocyclic amide bond is approximately orthogonal to the plane of the phenyl ring, making a dihedral angle of 82.31 (3°. The water molecule acts as an acceptor to the proton of the amino group in an N—H...O interaction, and as a double proton donor in O—H...O hydrogen bonds, generating infinite bands along the a axis.

  16. Spectroscopy Studying on Derivatives 2H-azepine [1,5] PrS- migration Reaction%2H-氮杂卓衍生物[1,5]迁移反应的光谱学特征

    Institute of Scientific and Technical Information of China (English)

    金月仙

    2009-01-01

    氮杂卓化合物存在1H-,2H-,3H-和4H-共4个互变异构体,其中,2H-,3H-系统是最重要的.2H-氮杂卓母体化合物很不稳定,4位存在叔-丁基,并且环上含有丙硫基(PrS-)取代基的2H-氮杂卓,不仅发生H迁移,也能发生PrS-迁移,向较稳定的3H-氮杂卓异构化.以2,7-二甲氧基-4-甲基-2H-氮杂卓为原料,通过与Pr-SH的取代反应,合成7-甲氧基-4-甲基-2-PrS-2H-氮杂卓,并讨论分析产物的[1,5]迁移反应.通过IR、1H NMR、13C NMR、MS检测表明,在室温条件下,4位存在甲基的2H-氮杂卓衍生物,选择性地发生[1,5]PrS-迁移,生成3H-氮杂卓,而且此异构化反应速度比叔-丁基存在时的情况更快.

  17. The identification of a novel phosphodiesterase 4 inhibitor, 1-ethyl-5-{5-[(4-methyl-1-piperazinyl)methyl]-1,3,4-oxadiazol-2-yl}-N-(tetrahydro-2H-pyran-4-yl)-1H-pyrazolo[3,4-b]pyridin-4-amine (EPPA-1), with improved therapeutic index using pica feeding in rats as a measure of emetogenicity.

    Science.gov (United States)

    Davis, T Gregg; Peterson, John J; Kou, Jen-Pyng; Capper-Spudich, Elizabeth A; Ball, Doug; Nials, Anthony T; Wiseman, Joanne; Solanke, Yemisi E; Lucas, Fiona S; Williamson, Richard A; Ferrari, Livia; Wren, Paul; Knowles, Richard G; Barnette, Mary S; Podolin, Patricia L

    2009-09-01

    Clinical utility of phosphodiesterase 4 (PDE4) inhibitors as anti-inflammatory agents has, to date, been limited by adverse effects including nausea and emesis, making accurate assessment of emetic versus anti-inflammatory potencies critical to the development of inhibitors with improved therapeutic indices. In the present study we determined the in vitro and in vivo anti-inflammatory potencies of the first-generation PDE4 inhibitor, rolipram, the second-generation inhibitors, roflumilast and cilomilast, and a novel third generation inhibitor, 1-ethyl-5-{5-[(4-methyl-1-piperazinyl)methyl]-1,3,4-oxadiazol-2-yl}-N-(tetrahydro-2H-pyran-4-yl)-1H-pyrazolo[3,4-b]pyridin-4-amine (EPPA-1). The rank-order potency against lipopolysaccharide (LPS)-induced tumor necrosis factor-alpha production by human peripheral blood mononuclear cells was roflumilast (IC(50) = 5 nM) > EPPA-1 (38) > rolipram (269) > cilomilast (389), and against LPS-induced pulmonary neutrophilia in the rat was EPPA-1 (D(50) = 0.042 mg/kg) > roflumilast (0.24) > rolipram (3.34) > cilomilast (4.54). Pica, the consumption of non-nutritive substances in response to gastrointestinal stress, was used as a surrogate measure for emesis, giving a rank-order potency of rolipram (D(50) = 0.495 mg/kg) > roflumilast (1.6) > cilomilast (6.4) > EPPA-1 (24.3). The low and high emetogenic activities of EPPA-1 and rolipram, respectively, detected in the pica model were confirmed in a second surrogate model of emesis, reversal of alpha(2)-adrenoceptor-mediated anesthesia in the mouse. The rank order of therapeutic indices derived in the rat [(pica D(50))/(neutrophilia D(50))] was EPPA-1 (578) > roflumilast (6.4) > cilomilast (1.4) > rolipram (0.15), consistent with the rank order derived in the ferret [(emesis D(50))/(neutrophilia D(50))]. These data validate rat pica feeding as a surrogate for PDE4 inhibitor-induced emesis in higher species, and identify EPPA-1 as a novel PDE4 inhibitor with an improved therapeutic index.

  18. Synthesis, Crystal Structure and Thermal Decomposition of [Ce(NO3)5H2O]·(C3N2H5)2%[Ce(NO3)5H2O]·(C3H5N2)2的合成、晶体结构及热分析

    Institute of Scientific and Technical Information of China (English)

    薛岗林; 杨一心; 李恒新; 何水样; 李君

    2001-01-01

    Colorless crystal,[Ce(NO3) 5H2O]·(C3N2H5)2, has been obtained from the reaction of Ce(NO3)3 with imdazole in the aqueous solution and its crystal structure has been determined by single crystal X-ray diffraction techniques. The crystal belongs to triclinic, space group P1. The cell parameters are: a=0.7489(1) nm, b=0.7914(2)nm, c=1.8139(3)nm, α=89.39(2)°, β=89.37(1)°, γ=63.18(2)°, Dc=2. lg·cm-3, Z=2, R=0.0319. In the compound, all of five nitrates are bidentate and one molecule of water is monodentate, the coordination number of Ce(Ⅲ) is 11.The processes of thermal decomposition of the compound was proposed by its TG curve.

  19. 4-(4-Methoxyphenyl-1-phenylpyridine-2,6(1H,3H-dione

    Directory of Open Access Journals (Sweden)

    Ushati Das

    2009-06-01

    Full Text Available In the title compound, C18H15NO3, the pyridine-2,6-dione ring adopts an envelope conformation. The phenyl ring lies approximately perpendicular to the mean plane of the pyridine-2,6-dione ring [dihedral angle = 81.5 (1°], while the methoxyphenyl ring is tilted to the same plane by a dihedral angle of 34.8 (1°. Intermolecular C—H...O interactions link the molecules into chains along [100].

  20. 1,3-Bis(4-methylbenzylpyrimidine-2,4(1H,3H-dione

    Directory of Open Access Journals (Sweden)

    Gong-Chun Li

    2010-01-01

    Full Text Available In the title molecule, C20H20N2O2, the central pyrimidine ring forms dihedral angles of 71.9 (1 and 69.8 (1° with the two benzene rings. In the crystal, weak intermolecular C—H...O hydrogen bonds link molecules into centrosymmetric dimers. The crystal packing exhibits also π–π interactions as indicated by short distances of 3.674 (2 Å between the centroids of the pyrimidine rings of neighbouring molecules.

  1. 1-Decyl-6-nitro-1H-benzimidazol-2(3H-one

    Directory of Open Access Journals (Sweden)

    Younes Ouzidan

    2011-11-01

    Full Text Available The title molecule, C17H25N3O3, is built up from fused six- and five-membered rings linked to a –C10H21 chain. The fused-ring system is essentially planar, the largest deviation from the mean plane being 0.009 (2 Å. The chain is roughly perpendicular to this plane, making a dihedral angle of 79.5 (2°. In the crystal, N—H...O hydrogen bonds build infinite chains along [010]. There are channels in the structure containing disordered hexane. The contribution of this solvent to the scattering power was suppressed using the SQUEEZE option in PLATON [Spek (2009. Acta Cryst. D65, 148–155].

  2. 5-Chloro-1-nonyl-1H-benzimidazol-2(3H-one

    Directory of Open Access Journals (Sweden)

    Youssef Kandri Rodi

    2011-12-01

    Full Text Available The asymmetric unit of the title compound, C16H23ClN2O, comtains two independent molecules in which the fused-ring systems are essentially planar, the largest deviation from the mean plane of each molecule being 0.011 (2 Å and 0.016 (2 Å. The benzimidazole rings of the two molecules make a dihedral angle of 66.65 (7°. The nonyl substituents are almost perpendicular to the benzimidazole planes [C—N—C—C tosrsion angles = 96.0 (3 and 81.0 (2°]. In the crystal, each independent molecule forms an inversion dimer via a pair of N—H...O hydrogen bonds. In one of the independent molecules, the terminal –CH2–CH3 group of the alkyl chain is disordered over two sets of sites with a refined occupancy ratio of 0.746 (7:0.254 (7.

  3. 1,3-Dibenzyl-1H-benzimidazol-2(3H-one

    Directory of Open Access Journals (Sweden)

    Youssef Kandri Rodi

    2011-12-01

    Full Text Available In the molecular structure of the title compound, C21H18N2O, the fused-ring system is essentially planar, the largest deviation from the mean plane being 0.0121 (9 Å. The O atom and adjacent C atom are located in Wyckoff position 4e on a twofold axis (0, y, 1/4. The two benzyl groups are almost perpendicular to the benzimidazole plane, but point in opposite directions. The dihedral angle between the benzimidazole mean plane and the phenyl ring is 81.95 (5°, whereas that between the two benzyl groups is 60.96 (7°.

  4. ГИДРОХИМИЧЕСКИЙ СИНТЕЗ СИЛИКАТОВ КАЛЬЦИЯ В СИСТЕМАХ CACL2-NA2SIO3-H2O, CASO4·2H2O-NA2SIO3-H2O, CASO4·2H2O-SIO2·NH2O-KOH. СОСТАВ, СТРУКТУРА, СВОЙСТВА

    OpenAIRE

    2009-01-01

    Представлены результаты исследования процессов гидрохимического синтеза силикатов кальция. Определены особенности кинетики синтеза силикатов кальция в системе CaSO4·2H2O-Na2SiO3-H2O. Изучены состав, структура и основные физико-химические свойства полученных силикатов кальция методами рентгенофазового, термогравиметрического анализа, инфракрасной спектроскопии, сканирующей электронной и атомносиловой микроскопии....

  5. Synthesis, X-ray Single Crystal Structure, Molecular Docking and DFT Computations on N-[(1E-1-(2H-1,3-Benzodioxol-5-yl-3-(1H-imidazol-1-ylpropylidene]-hydroxylamine: A New Potential Antifungal Agent Precursor

    Directory of Open Access Journals (Sweden)

    Reem I. Al-Wabli

    2017-02-01

    Full Text Available Mycoses are serious health problem, especially in immunocompromised individuals. A new imidazole-bearing compound containing an oxime functionality was synthesized and characterized with different spectroscopic techniques to be used for the preparation of new antifungal agents. The stereochemistry of the oxime double bond was unequivocally determined via the single crystal X-ray technique. The title compound 4, C13H13N3O3·C3H8O, crystallizes in the monoclinic space group P21with a = 9.0963(3 Å, b = 14.7244(6 Å, c = 10.7035(4 Å, β = 94.298 (3°, V = 1429.57(9 Å3, Z = 2. The molecules were packed in the crystal structure by eight intermolecular hydrogen bond interactions. A comprehensive spectral analysis of the title molecule 4 has been performed based on the scaled quantum mechanical (SQM force field obtained by density-functional theory (DFT calculations. A molecular docking study illustrated the binding mode of the title compound 4 into its target protein. The preliminary antifungal activity of the title compound 4 was determined using a broth microdilution assay.

  6. UV/vis, 1H, and 13C NMR spectroscopic studies to determine mangiferin p Ka values

    Science.gov (United States)

    Gómez-Zaleta, Berenice; Ramírez-Silva, María Teresa; Gutiérrez, Atilano; González-Vergara, Enrique; Güizado-Rodríguez, Marisol; Rojas-Hernández, Alberto

    2006-07-01

    The acid constants of mangiferin (a natural xanthonoid) in aqueous solution were determined through an UV/vis spectroscopic study employing the SQUAD program as a computational tool. A NMR study complements the p Ka values assignment and evidences a H-bridge presence on 1-C. The chemical model used was consistent with the experimental data obtained. The p Ka values determined with this procedure were as follows: H 4(MGF) = H 3(MGF) - + H +, pK(6-H) = 6.52 ± 0.06; H 3(MGF) - = H 2(MGF) 2- + H +, pK(3-H) = 7.97 ± 0.06; H 2(MGF) 2- = H(MGF) 3- + H +, pK(7-H) = 9.44 ± 0.04; H(MGF) 3- = (MGF) 4- + H +, pK(1-H) = 12.10 ± 0.01; where it has been considered mangiferin C 19H 18O 11 as H 4(MGF). Mangiferin UV/vis spectral behavior, stability study in aqueous solution as well as NMR spectroscopy studies: one-dimensional 1H, 13C, 2D correlated 1H/ 13C performed by (g)-HSQC and (g)-HMBC methods; are also presented. p Ka values determination of H 4(MGF) in aqueous solution is a necessary contribution to subsequent pharmacokinetic study, and a step towards the understanding of its biological effects.

  7. Aquabis(3,5-dimethyl-1H-pyrazole-kappaN2)(malonato-kappa2O,O')copper(II) dihydrate.

    Science.gov (United States)

    Xiong, Y; Tong, M; An, T; Karlsson, H T

    2001-12-01

    In the neutral title complex, [Cu(C3H2O4)(C5H8N2)2(H2O)]*2H2O or [Cu(mal)(dmp)2(H2O)]*2H2O (mal is malonate and dmp is 3,5-dimethyl-1H-pyrazole), the Cu(II) ion, in a slightly distorted square-pyramidal geometry, is coordinated by two O atoms of the bidentate malonate, the O atom of the water ligand and two N atoms from the two 3,5-dimethylpyrazole ligands. The mean Cu-N bond length is 2.007 (6) A, longer than the Cu-O(mal) bonds [1.950 (5) A]. The apical position is occupied by a relatively strongly coordinated water molecule [Cu-O(water) 2.288 (5) A]. The crystal structure is characterized by the layer motif of a hydrogen-bonded network.

  8. Changes of GABA A Receptor α1 Subunit mRNA and [3H] Flunirazepam Binding in Animal Model of Status Epileptic Rats

    Institute of Scientific and Technical Information of China (English)

    Qinchi Lu

    2000-01-01

    OBJECTIVE: In the present study, we determinded whether status epilepticus or prolonged limbic seizures ( induced by pilocarpine) altered GABA A receptor αl subunit gene expression m the hippocanpus. BACKGROUND: A decrease in GABAergic inhibition during epileptogenesis plays an imprortant role in the development of persistent hyperexcitability observed during chronic epilepsy. METHODS: Stares epilepticus was reduced in male adult rats by a single i.p. injection ofpilocarpine (320-340 mg/kg). Rats that survived status epilepticus ( definded as continous seizure activity in the EcoG for at least 40 min) for 1 h and 2 h were sacrificed for GABA A receptor gene expression and binding assay. In situ hybridization was used to measure regional mRNA levels, and [3H] flunirazepam used to label the benzodiazepine binding sites. RESULTS: We found that 2h after the onset of seizure, GABA A receptor α1 m RNA decresed significarntly in the CA1 and CA3 fields of hippocampus. No significant change in ctl mRNA was observed in the dentate gyrus. However, [3H] flunirazepam binding decreased uniformly in CA l, CA3 and dentate gyrus 2h after status epfileptius. 1 h ofcontinuous seizures did not produce any significant change in either αl mRNA or [3H] flunirazepam birding in any of the hippocampal regions studied. Cresyl violet staining of the brain hippocampus areas lh or 2h after the seizure-onset. DISCUSSION: The above changes make the brain more susceptible for the development of chronic epilepsy. CONCLUSION: These results suggest that status epilepticus-induced decreased in GABA A recepor αl gene expression and [3H] flunirazepam binding in the hippocampus.

  9. A Cu (NO3)2.3H2O catalysed facile synthesis of substituted 4(3H)-quinazolinones and benzimidazoles

    Indian Academy of Sciences (India)

    G A N K Durgareddy; R Ravikumar; S Ravi; Srinivas R Adapa

    2013-01-01

    One pot synthesis of alkyl, aryl, heteroaryl mono(2)substituted 4(3H)-quinazolinones and 2-aryl or heteroaryl, 1-arylmethyl or heteroarylmethyl -1H-benzimidazoles using a water soluble Cu (NO3)2.3H2O catalyst at room/ambient temperature in excellent yield.

  10. 1H and 13C NMR study of perdeuterated pyrazoles

    OpenAIRE

    Jimeno, María Luisa; Jagerovic, Nadine; Elguero, José; Junk, Thomas; Catallo, W. James

    1997-01-01

    The 1H and 13C chemical shifts as well as the 1H–2H and 2H–13C coupling constants of perdeuterated 3,5-dimethylpyrazole and 3,5-diphenylpyrazole have been measured and the values compared with those of the unlabelled compounds.

  11. Role of cluster size and substrate in the gas phase CC bond coupling reactions of allyl halides mediated by Agn+ and Agn-1H+ cluster cations

    Science.gov (United States)

    Wang, Farrah Qiuyun; Khairallah, George N.; O'Hair, Richard A. J.

    2009-06-01

    Previous studies have demonstrated that the silver hydride cluster cation Ag4H+ promotes CC bond coupling of allylbromide [G.N. Khairallah, R.A.J. O'Hair, Angewandte Chemie International Edition 44 (2005) 728]. Here the influence of both the nature and the size of the silver cluster cation and the substrate on CC bond coupling are examined. Thus each of the cations Ag2H+, Ag4H+, Ag3+, and Ag5+ were allowed to react with three different halides: allyl chloride, allyl bromide and allyl iodide. No CC bond coupling is observed in the reactions of the cluster cations with allyl chloride. There are four main reaction sequences that result in CC bond coupling for allyl bromide and allyl iodide mediated by Agn+ and Agn-1H+ clusters: (i) A sequence involving the reactions of silver cluster cations with two molecules of C3H5X: Agn+ --> Agn(C3H5X)+ --> AgnX2+. This only occurs in the cases of: n = 3 and X = I; n = 5 and X = Br. (ii) A sequence involving the reactions of silver cluster cations with two molecules of C3H5X via an organometallic intermediate: Agn+ --> Agn-1(C3H5)+ --> Agn-1X+. This only occurs in the cases of: n = 5 and X = Br and I. (iii) A sequence involving the reactions of silver hydride cluster cations with three molecules of C3H5X: Agn-1H+ --> Agn-1X+ --> Agn-1X(C3H5X)+ --> Ag(C3H5)2+ and Agn-1X3+. This only occurs in the cases of: n = 5 and X = Br and I. (iv) A sequence involving the reactions of silver hydride cluster cations with three molecules of C3H5X via an organometallic intermediate: Agn-1H+ --> Agn-1X+ --> Agn-3(C3H5)+ --> Ag(C3H5)2+ and Agn-3X+. This only occurs in the cases of: n = 5 and X = I.

  12. Synthesis, reactions and biological activity of 3-arylidene-5-(4-methylphenyl-2(3H-furanones

    Directory of Open Access Journals (Sweden)

    ASIF HUSAIN

    2009-02-01

    Full Text Available 3-Arylidene-5-(4-methylphenyl-2(3H-furanones 2a–m were prepared from 3-(4-methyl-benzoylpropanoic acid 1 and several aromatic aldehydes. Some of the selected furanones were reacted with ammonia gas and benzylamine to give corresponding 3-arylidene-1,3-dihydro-5-(4-methylphenyl-2H-pyrrol-2-ones 3a–h and 3-arylidene-1-benzyl-1,3-dihydro-5-(4-methylphenyl-2H-pyrrol-2-ones 4a–f, respectively, which were characterized on the basis of IR, 1H-NMR, mass spectral data and elemental analysis results. These compounds were tested for their anti-inflammatory and antibacterial activities. The compounds, which showed significant anti-inflammatory activity, were further screened for their analgesic and ulcerogenic activities. Three new compounds (2e, 2h and 4d, out of twenty-seven showed very good anti-inflammatory activity in the carrageenan induced rat paw edema test, with significant analgesic activity in the acetic acid induced writhing test together with negligible ulcerogenic action. The antibacterial activity is expressed as the corresponding MIC values.

  13. Synthesis of ( sup 3 H)naltrindole

    Energy Technology Data Exchange (ETDEWEB)

    Dorn, C.R.; Markos, C.S.; Dappen, M.S.; Pitzele, B.S. (Searle (G.D.) and Co., Skokie, IL (United States). R and D Div.)

    1992-05-01

    ({sup 3}H)Naltrindole (({sup 3}H)1) was prepared for use as a selective radiolabeled ligand for delta opioid receptors. The Fischer indole synthesis from naltrexone and 2,4-dibromophenylhydrazine produced dibromide precursor 2, which was catalytically dehalogenated with carrier free tritium gas to afford ({sup 3}H)1 in 45.8% yield at a specific activity of 39.5 Ci/mmol. (author).

  14. Immobilization of Ag(i) into a metal-organic framework with -SO3H sites for highly selective olefin-paraffin separation at room temperature.

    Science.gov (United States)

    Chang, Ganggang; Huang, Minhui; Su, Ye; Xing, Huabin; Su, Baogen; Zhang, Zhiguo; Yang, Qiwei; Yang, Yiwen; Ren, Qilong; Bao, Zongbi; Chen, Banglin

    2015-02-18

    Introduction of Ag(i) ions into a sulfonic acid functionalized MOF ((Cr)-MIL-101-SO3H) significantly enhances its interactions with olefin double bonds, leading to its much higher selectivities for the separation of C2H4-C2H6 and C3H6-C3H8 at room temperature over the original (Cr)-MIL-101-SO3H and other adsorbents at room temperature.

  15. Thermodynamic study of (alkyl esters + {alpha},{omega}-alkyl dihalides) VII. H{sub m}{sup E} and V{sub m}{sup E} for 20 binary mixtures {l_brace}xC{sub u-1}H{sub 2u-1}CO{sub 2}C{sub 3}H{sub 7} + (1 - x){alpha},{omega}-ClCH{sub 2}(CH{sub 2}){sub v-2}CH{sub 2}Cl{r_brace}, where u = 1 to 4, {alpha} = 1 and v = {omega} = 2 to 6. An analysis of behavior using the COSMO-RS methodology

    Energy Technology Data Exchange (ETDEWEB)

    Marrero, E. [Laboratorio de Termodinamica y Fisicoquimica de Fluidos (www.thermo.ulpgc.es), Parque Cientifico-Tecnologico, Campus Universitario de Tafira, Universidad de Las Palmas de Gran Canaria, 35071 Las Palmas de Gran Canaria, Canary Islands (Spain); Ortega, J. [Laboratorio de Termodinamica y Fisicoquimica de Fluidos (www.thermo.ulpgc.es), Parque Cientifico-Tecnologico, Campus Universitario de Tafira, Universidad de Las Palmas de Gran Canaria, 35071 Las Palmas de Gran Canaria, Canary Islands (Spain)], E-mail: jortega@dip.ulpgc.es; Palomar, J. [Seccion de Ingenieria Quimica, Dpto. de Quimica-Fisica Aplicada, Universidad Autonoma de Madrid, Cantoblanco, 28049 Madrid (Spain)

    2009-03-15

    Summary: Excess enthalpies H{sub m}{sup E} and excess volumes V{sub m}{sup E} obtained at a temperature of 298.15 K and atmospheric pressure are presented for a set of 20 binary mixtures comprised of the first four propyl esters, C{sub u-1}H{sub 2u-1}COOC{sub 3}H{sub 7} (u = 1 to 4), and five {alpha},{omega}-dichloroalkanes, ClCH{sub 2}(CH{sub 2}){sub v-2}CH{sub 2}Cl (v = 2 to 6). All the mixtures are exothermic except for those corresponding to propyl methanoate with v {>=} 4. The V{sub m}{sup E} are positive in most mixtures except for those where v = 4, 5, 6, for V{sub m}{sup E}<0. There is a regular rise in H{sub m}{sup E} with v, while the increase in u produces a greater exothermicity in the mixing process, which becomes inverted for propyl butanoate. The variation in V{sub m}{sup E} with the chain length of the compounds of the mixtures studied is not regular since both the enthalpic and the volumetric effects are due to interactions of different nature, positive and negative. Interpretation of the behavior was assisted by applying the quantum-chemistry method COSMO-RS. This method describes qualitatively and quantitatively the contribution of the different types of interactions, electrostatic, van der Waals, and those due to the (Cl, Cl) bond in the dihalide, and the influence of the ester and dichloroalkane chains. This information was also useful to adequately modify the application of the UNIFAC group contribution model, proposing parameters for the Cl, Cl/carboxylate interaction that vary with the chain length of the compounds involved. With this modification, the results estimated by UNIFAC model can be considered good.

  16. Nuclear Magnetic Resonance (NMR), Infrared (IR) and Mass Spectrometry (MS) study of keto-enol tautomerism of isobenzofuran-1(3H)-one derivatives

    Science.gov (United States)

    Pires, Diego Arantes Teixeira; Pereira, Wagner Luiz; Teixeira, Róbson Ricardo; Figueroa-Villar, José Daniel; Nascimento, Claudia Jorge do

    2016-06-01

    The keto-enol tautomerism of 3-(2-hydroxy-4,4-dimethyl-6-oxo-cyclohexen-1-yl)isobenzofuran-1(3H-one (1), 3-(2-hydroxy-6-oxocyclohex-1-enyl)isobenzofuran-1(3H)-one (2), 3-(2-hydroxy-4-methyl-6-oxocyclohex-1-enyl)isobenzofuran-1(3H)-one (3), 3-(2-hydroxy-5-oxocyclopent-1-enyl)isobenzofuran-1(3H)-one (4) and 2-(3-oxo-1,3-dihydroisobenzofuran-1-yl)-1H-indene-1,3(2H)-dione (5) were investigated. We noticed that for compounds 1 to 4 only the enol form is observed in solid, in solution or in the gas phase. Their tautomeric equilibria are not affected by the solvent, temperature or physical state. Compound 5 was observed in its keto form in solution (NMR) and solid state (IR). The enol species of 5 was also observed upon Mass Spectrometry analysis. These findings were supported by NMR, IR, MS/MS and molecular modeling analyses.

  17. Mild hydration of didecyldimethylammonium chloride modified DNA by 1H-nuclear magnetic resonance and by sorption isotherm

    Science.gov (United States)

    Harańczyk, H.; Kobierski, J.; Nizioł, J.; Hebda, E.; Pielichowski, J.; Zalitacz, D.; Marzec, M.; El-Ghayoury, A.

    2013-01-01

    The gaseous phase hydration of deoxyribonucleic acid and didecyldimethylammonium chloride (C19H42ClN) complexes (DNA-DDCA) was observed using hydration kinetics, sorption isotherm, and high power nuclear magnetic resonance. Three bound water fractions were distinguished: (i) a very tightly bound water not removed by incubation over silica gel, (ii) a tightly bound water saturating with the hydration time t1h = (0.59 ± 0.04) h, and a loosely bound water fraction, (iii) with the hydration time t2h = (20.9 ± 1.3) h. Proton free induction decay was decomposed into the signal associated with the solid matrix of DNA-DDCA complex (T2S∗≈ 30 μs) and two liquid signal components coming from tightly bound (T2L1∗≈ 100 μs) and from loosely bound water fraction (T2L2∗≈ 1000 μs).

  18. The interstellar chemistry of C3H and C3H2 isomers

    Science.gov (United States)

    Loison, Jean-Christophe; Agúndez, Marcelino; Wakelam, Valentine; Roueff, Evelyne; Gratier, Pierre; Marcelino, Núria; Reyes, Dianailys Nuñez; Cernicharo, José; Gerin, Maryvonne

    2017-10-01

    We report the detection of linear and cyclic isomers of C3H and C3H2 towards various starless cores and review the corresponding chemical pathways involving neutral (C3Hx with x = 1,2) and ionic (C3Hx+ with x = 1,2,3) isomers. We highlight the role of the branching ratio of electronic dissociative recombination (DR) reactions of C3H2+ and C3H3+ isomers, showing that the statistical treatment of the relaxation of C3H* and C3H2* produced in these DR reactions may explain the relative c,l-C3H and c,l-C3H2 abundances. We have also introduced in the model the third isomer of C3H2 (HCCCH). The observed cyclic-to-linear C3H2 ratio varies from 110 ± 30 for molecular clouds with a total density of about 1 × 104 molecules cm-3 to 30 ± 10 for molecular clouds with a total density of about 4 × 105 molecules cm-3, a trend well reproduced with our updated model. The higher ratio for molecular clouds with low densities is determined mainly by the importance of the H + l-C3H2 → H + c-C3H2 and H + t-C3H2 → H + c-C3H2 isomerization reactions.

  19. Influence of local molecular motions on the determination of 1H-1H internuclear distances measured by 2D 1H spin-exchange experiments.

    Science.gov (United States)

    Brus, J; Petrícková, H; Dybal, J

    2003-06-01

    Analysis of spin-exchange build-up curves obtained by measurement of 2D 1H CRAMPS spectra of alpha-glycine was performed to evaluate the rate of 1H-1H spin-exchange process with respect to the influence of variation in internal molecular motion. Differences in local motions significantly affect spin-exchange constants even in highly rigid organic solids with virtually uniform motion behavior. The polarization transfer between nonequivalent alpha-protons is described by the spin-exchange constant D=0.77 nm(2)ms(-1), while the polarization transfer involving spin exchange between alphaH and NH(3)(+) protons is characterized by D=0.24-0.21 nm(2)ms(-1). This significant decrease corresponds to rotation of hydrogen-bonded amino groups. Neglecting this variation in local spin-exchange constants the resulting calculated 1H-1H distance can be overestimated by up to 100%. Complications following from relayed and back polarization transfer involving the nearest spins within one functional group (e.g., CH(2) and/or NH(3)(+)) and intermolecular spin exchange are discussed. It was shown that 2H quadrupolar splitting determined for selected sites directly correlates with the experimentally observed differences in spin-exchange coefficients. It is also demonstrated that a medium level quantum chemical calculation of molecular dynamics provides relevant data that can be used to estimate differences in molecular motions.

  20. Reference: OCTAMERMOTIFTAH3H4 [PLACE

    Lifescience Database Archive (English)

    Full Text Available OCTAMERMOTIFTAH3H4 Nakayama T, Sakamoto A, Yang P, Minami M, Fujimoto Y, Ito T, Iwa...buchi M Highly conserved hexamer, octamer and nonamer motifs are positive cis-regulatory elements of the whe

  1. Decreased insulin clearance in individuals with elevated 1-h post-load plasma glucose levels.

    Directory of Open Access Journals (Sweden)

    Maria Adelaide Marini

    Full Text Available Reduced insulin clearance has been shown to predict the development of type 2 diabetes. Recently, it has been suggested that plasma glucose concentrations ≥ 8.6 mmol/l (155 mg/dl at 1 h during an oral glucose tolerance test (OGTT can identify individuals at high risk for type 2 diabetes among those who have normal glucose tolerance (NGT 1 h-high. The aim of this study was to examine whether NGT 1 h-high have a decrease in insulin clearance, as compared with NGT individuals with 1-h post-load glucose <8.6 mmol/l (l (155 mg/dl, NGT 1 h-low. To this end, 438 non-diabetic White individuals were subjected to OGTT and euglycemic-hyperinsulinemic clamp to evaluate insulin clearance and insulin sensitivity. As compared with NGT 1 h-low individuals, NGT 1 h-high had significantly higher 1-h and 2-h post-load plasma glucose and 2-h insulin levels as well as higher fasting glucose and insulin levels. NGT 1 h-high exhibited also a significant decrease in both insulin sensitivity (P<0.0001 and insulin clearance (P = 0.006 after adjusting for age, gender, adiposity measures, and insulin sensitivity. The differences in insulin clearance remained significant after adjustment for fasting glucose (P = 0.02 in addition to gender, age, and BMI. In univariate analyses adjusted for gender and age, insulin clearance was inversely correlated with body weight, body mass index, waist, fat mass, 1-h and 2-h post-load glucose levels, fasting, 1-h and 2-h post-load insulin levels, and insulin-stimulated glucose disposal. In conclusion, our data show that NGT 1 h-high have a reduction in insulin clearance as compared with NGT 1 h-low individuals; this suggests that impaired insulin clearance may contribute to sustained fasting and post-meal hyperinsulinemia.

  2. 5-Chloro-1-[(E-3-(dimethylaminoacryloyl]-3-methyl-1H-benzimidazol-2(3H-one–6-chloro-1-[(E-3-(dimethylaminoacryloyl]-3-methyl-1H-benzimidazol-2(3H-one (4/1

    Directory of Open Access Journals (Sweden)

    Rachida Dardouri

    2011-07-01

    Full Text Available In the reaction of 7-chloro-1,5-benzodiazepine-2,4-dione with N,N-dimethylformamide/dimethylacetal, the diazepine seven-membered ring undergoes a contraction to form the five-membered ring. The reaction yields two isomers the title compound, C13H14ClN3O2; the major component has the chlorine-atom substituent in the 5-position of the benzimidazolone ring and the minor component has the chlorine atom in the 6-position. The two isomers form a disordered co-crystal, the chloromethylbenzimidazolone portion of both components are disordered with respect to each other in a 4:1 ratio [the refined ratio is 0.816 (5:0.184 (5]; the dimethylaminocryloyl substitutent is ordered. The double bond of the dimethylaminoacryloyl substituent has an E configuration.

  3. Hydrogen dynamics in soil organic matter as determined by 13C and 2H labeling experiments

    Science.gov (United States)

    Paul, Alexia; Hatté, Christine; Pastor, Lucie; Thiry, Yves; Siclet, Françoise; Balesdent, Jérôme

    2016-12-01

    Understanding hydrogen dynamics in soil organic matter is important to predict the fate of 3H in terrestrial environments. One way to determine hydrogen fate and to point out processes is to examine the isotopic signature of the element in soil. However, the non-exchangeable hydrogen isotopic signal in soil is complex and depends on the fate of organic compounds and microbial biosyntheses that incorporate water-derived hydrogen. To decipher this complex system and to understand the close link between hydrogen and carbon cycles, we followed labeled hydrogen and labeled carbon throughout near-natural soil incubations. We performed incubation experiments with three labeling conditions: 1 - 13C2H double-labeled molecules in the presence of 1H2O; 2 - 13C-labeled molecules in the presence of 2H2O; 3 - no molecule addition in the presence of 2H2O. The preservation of substrate-derived hydrogen after 1 year of incubation (ca. 5 % in most cases) was lower than the preservation of substrate-derived carbon (30 % in average). We highlighted that 70 % of the C-H bonds are broken during the degradation of the molecule, which permits the exchange with water hydrogen. Added molecules are used more for trophic resources. The isotopic composition of the non-exchangeable hydrogen was mainly driven by the incorporation of water hydrogen during microbial biosynthesis. It is linearly correlated with the amount of carbon that is degraded in the soil. The quantitative incorporation of water hydrogen in bulk material and lipids demonstrates that non-exchangeable hydrogen exists in both organic and mineral-bound forms. The proportion of the latter depends on soil type and minerals. This experiment quantified the processes affecting the isotopic composition of non-exchangeable hydrogen, and the results can be used to predict the fate of tritium in the ecosystem or the water deuterium signature in organic matter.

  4. An oxazolo[3,2-b]indazole route to 1H-indazolones.

    Science.gov (United States)

    Oakdale, James S; Solano, Danielle M; Fettinger, James C; Haddadin, Makhluf J; Kurth, Mark J

    2009-07-02

    The novel heterocycle 2,3-dihydrooxazolo[3,2-b]indazole has been synthesized and utilized to provide easy access to 1H-indazolones, particularly the previously unreported 2-(2-alkoxyethyl)-1H-indazol-3(2H)-ones. Mechanistic as well as optimization and reaction scope studies are reported.

  5. (E-3-[(Dimethylaminomethylidene]-4-phenyl-1H-1,5-benzodiazepin-2(3H-one

    Directory of Open Access Journals (Sweden)

    Mohamed Loughzail

    2014-02-01

    Full Text Available The asymmetric unit of the title compound, C18H17N3O, consists of two independent molecules, each having an E conformation with respect to the C=C bond between the benzodiazepinone and dimethylamine groups. In the crystal, the two independent molecules are linked into a dimer by a pair of N—H...O hydrogen bonds.

  6. Pelanserin: 3-[3-(4-phenylpiperazin-1-ylpropyl]quinazoline-2,4(1H,3H-dione

    Directory of Open Access Journals (Sweden)

    Gerardo Aguirre Hernández

    2014-08-01

    Full Text Available The title compound, C21H24N4O2, is a potent serotonin 5-HT2 and α1-adrenoceptor antagonist. The n-propyl chain links the quinazolinedione heterocycle and the phenylpiperazine group in which the benzene ring is equatorially located and the piperazine ring has the expected chair conformation. The dihedral angle between the planes of the benzene ring and the quinazolinedione ring system is 74.1 (1°. In the crystal, molecules form centrosymmetric dimers through R22(8 hydrogen-bonded rings involving the amine and one carbonyl group of the quinazolinedione moiety. These dimers are extended into chains extending along the a-axis direction through expanded centrosymmetric cyclic C—H...O associations involving the second carbonyl group, giving R22(20 and R12(7 motifs.

  7. 1-Methyl-1H-2,1-benzothiazin-4(3H-one 2,2-dioxide

    Directory of Open Access Journals (Sweden)

    Muhammad Nadeem Arshad

    2008-03-01

    Full Text Available In the crystal structure of the title compound, C9H9NO3S, there is distorted tetrahedral geometry around the S atom. The sulfonyl group is almost normal to the benzene ring, while the carbonyl O atom and methyl C atom are on opposite sides of this ring. The heterocyclic ring adopts a half-boat conformation with the S atom out of the plane. The molecules are dimerized by hydrogen bonding involving the benzene ring and the sulfonyl group. These dimers are linked to each other in the same way. There is an intramolecular hydrogen bond between a methyl C—H group and a sulfonyl O atom, and a π–π interaction between the aromatic rings of two dimers at a centroid-to-centroid distance of 3.6373 (13 Å.

  8. 1,3-Bis(3-phenylpropyl-1H-1,3-benzimidazole-2(3H-selone

    Directory of Open Access Journals (Sweden)

    Mehmet Akkurt

    2011-05-01

    Full Text Available The title molecule, C25H26N2Se, has mirror symmetry, with the mirror plane passing through the atoms of the C=Se bond and the mid-points of the two C—C bonds of the benzene ring of the benzimidazole group. The dihedral angle between the benzimidazole ring system and the phenyl ring is 71.62 (14°.

  9. Main: 1H49 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H49 トウモロコシ Corn Zea mays L. Beta-Glucosidase, Chloroplast Precursor Name=Glu1; Zea...NPWIYMYPEGLKDLLMIMKNKYGNPPIYITENGIGDVDTKETPLPMEAALNDYKRLDYIQRHIATLKESIDLGSNVQGYFAWSLLDNFEWFAGFTERYGIVYVDRNNNCTRYMKESAKWLKEFNTAKKPSKKILTPA corn_1H49.jpg ...

  10. Main: 1H81 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H81 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...PEGKGREFFLYASSRRGYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H81.jpg ...

  11. Main: 1H86 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H86 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...PEGKGREFFLYASSRRGYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H86.jpg ...

  12. Main: 1H84 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H84 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...GYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H84.jpg ...

  13. Main: 1H83 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H83 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...GYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H83.jpg ...

  14. Main: 1H82 [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H82 トウモロコシ Corn Zea mays L. Polyamine Oxidase Precursor Name=Pao; Zea Mays Molecul...PEGKGREFFLYASSRRGYYGVWQEFEKQYPDANVLLVTVTDEESRRIEQQSDEQTKAEIMQVLRKMFPGKDVPDATDILVPRWWSDRFYKGTFSNWPVGVNRYEYDQLRAPVGRVYFTGEHTSEHYNGYVHGAYLSGIDSAEILINCAQKKMCKYHVQGKYD corn_1H82.jpg ...

  15. Reference: OCTAMERMOTIFTAH3H4 [PLACE

    Lifescience Database Archive (English)

    Full Text Available OCTAMERMOTIFTAH3H4 Taoka K, Kaya H, Nakayama T, Araki T, Meshi T, Iwabuchi M Identi...fication of three Kinds of mutually related composite elements conferring S phase-specific transcriptional activation Plant J 18:611-623 (1999) PubMed: 10417712; ...

  16. 3H-labelling of myo-inositol at L-C1 minimizes aberrant 3H in nucleotides

    DEFF Research Database (Denmark)

    Christensen, Søren; Jensen, Annelie Kolbjørn; Simonsen, L.O.

    2002-01-01

    aberrant K3H-labelling, inositol phosphate signalling, (3H)myo-inositol labelling, myo-inositol metabolism......aberrant K3H-labelling, inositol phosphate signalling, (3H)myo-inositol labelling, myo-inositol metabolism...

  17. Fragmentation Mechanism for A Group of 2(1H)-Quinoxalines%一类2(1H)-喹喔啉化合物的裂解机理

    Institute of Scientific and Technical Information of China (English)

    杨小兵; 丁松涛; 王安邦; 李小银; 杨裕生; 胡伟华

    2002-01-01

    用电子轰击质谱(EI-MS)研究了一类喹喔啉化合物:1-烷基-3-甲基-2(1H)-喹喔啉-2-酮(1-alkyl-3-methyl-2(1H)-quinoxalin-2-one,简称AMQ,其中alkyl=H,CH3,C2H5,n-C3H7,n-C5H11,n-C16H33);结果表明随着烷基链的增长,样品熔点通常会有所降低,结合在电子轰击下所产生的裂解碎片离子,并根据其结构特征以乙基化样品为代表,推导了该类化合物在电子轰击作用下可能发生的裂解机理.

  18. Main: OCTAMERMOTIFTAH3H4 [PLACE

    Lifescience Database Archive (English)

    Full Text Available OCTAMERMOTIFTAH3H4 S000076 11-May-2006 (last modified) kehi Octamer motif found in ...promoter of wheat (T.a.) histone genes H3 and H4, and corn histone genes H3 and H4; Arabidopsis histone H4; histone-specific oct...amer; About half of the Oct motifs are present together with another element, HexA, TCA ...or CCAAT-box, forming OCES (Oct-containing composite elements); histone; Oct; S-p

  19. KBS-3H design description 2005

    Energy Technology Data Exchange (ETDEWEB)

    Autio, Jorma (Saanio and Riekkola Oy, Helsinki (Finland))

    2008-05-15

    SKB and Posiva are performing an RandD program over the period of 2002-2007 with the overall aim to develop the KBS-3H to an alternative to the KBS-3V concept for disposal of spent nuclear fuel. A feasibility study of the KBS-3H concept was carried out in 2002, followed by the setting up of basic design in 2003. Several problems related to the behavior of the design and scope of future research and development work were addressed. Therefore the design basis was developed further and two candidate designs were developed: 1) previous Basic Design (BD) was developed more robust and tolerable to inflows. Parallel to that a novel modified 2) DAWE design with Drainage, Air evacuation and Watering and was developed to function robustly at various inflow situations. The candidate designs presented in this report include several novel components, such as fixing rings and steel plugs which have been designed without support of applicable design guidelines, regulations or standards available. The design basis and performance of these components include uncertainties, which should be studied and verified. It is possible that a feasible site specific design can be based on using both alternatives

  20. Galápagos hydroclimate of the Common Era from paired microalgal and mangrove biomarker 2H/1H values

    Science.gov (United States)

    Nelson, Daniel B.; Sachs, Julian P.

    2016-03-01

    Tropical maritime precipitation affects global atmospheric circulation, influencing storm tracks and the size and location of subtropical deserts. Paleoclimate evidence suggests centuries-long changes in rainfall in the tropical Pacific over the past 2,000 y, but these remain poorly characterized across most of the ocean where long, continuous proxy records capable of resolving decadal-to-centennial climate changes are still virtually nonexistent despite substantial efforts to develop them. Here we apply a new climate proxy based on paired hydrogen isotope ratios from microalgal and mangrove-derived sedimentary lipids in the Galápagos to reconstruct maritime precipitation changes during the Common Era. We show that increased rainfall during the Little Ice Age (LIA) (∼1400-1850 CE) was likely caused by a southward migration of the Intertropical Convergence Zone (ITCZ), and that this shift occurred later than previously recognized, coeval with dynamically linked precipitation changes in South America and the western tropical Pacific. Before the LIA, we show that drier conditions at the onset of the Medieval Warm Period (∼800-1300 CE) and wetter conditions ca. 2 ka were caused by changes in the El Niño/Southern Oscillation (ENSO). Collectively, the large natural variations in tropical rainfall we detect, each linked to a multicentury perturbation of either ENSO-like variability or the ITCZ, imply a high sensitivity of tropical Pacific rainfall to climate forcings.

  1. Galápagos hydroclimate of the Common Era from paired microalgal and mangrove biomarker 2H/1H values.

    Science.gov (United States)

    Nelson, Daniel B; Sachs, Julian P

    2016-03-29

    Tropical maritime precipitation affects global atmospheric circulation, influencing storm tracks and the size and location of subtropical deserts. Paleoclimate evidence suggests centuries-long changes in rainfall in the tropical Pacific over the past 2,000 y, but these remain poorly characterized across most of the ocean where long, continuous proxy records capable of resolving decadal-to-centennial climate changes are still virtually nonexistent despite substantial efforts to develop them. Here we apply a new climate proxy based on paired hydrogen isotope ratios from microalgal and mangrove-derived sedimentary lipids in the Galápagos to reconstruct maritime precipitation changes during the Common Era. We show that increased rainfall during the Little Ice Age (LIA) (∼1400-1850 CE) was likely caused by a southward migration of the Intertropical Convergence Zone (ITCZ), and that this shift occurred later than previously recognized, coeval with dynamically linked precipitation changes in South America and the western tropical Pacific. Before the LIA, we show that drier conditions at the onset of the Medieval Warm Period (∼800-1300 CE) and wetter conditions ca. 2 ka were caused by changes in the El Niño/Southern Oscillation (ENSO). Collectively, the large natural variations in tropical rainfall we detect, each linked to a multicentury perturbation of either ENSO-like variability or the ITCZ, imply a high sensitivity of tropical Pacific rainfall to climate forcings.

  2. [3H]Ethynylbicycloorthobenzoate ([3H]EBOB) binding in recombinant GABAA receptors.

    Science.gov (United States)

    Yagle, Monica A; Martin, Michael W; de Fiebre, Christopher M; de Fiebre, NancyEllen C; Drewe, John A; Dillon, Glenn H

    2003-12-01

    Ethynylbicycloorthobenzoate (EBOB) is a recently developed ligand that binds to the convulsant site of the GABAA receptor. While a few studies have examined the binding of [3H]EBOB in vertebrate brain tissue and insect preparations, none have examined [3H]EBOB binding in preparations that express known configurations of the GABAA receptor. We have thus examined [3H]EBOB binding in HEK293 cells stably expressing human alpha1beta2gamma2 and alpha2beta2gamma2 GABAA receptors, and the effects of CNS convulsants on its binding. The ability of the CNS convulsants to displace the prototypical convulsant site ligand, [35S]TBPS, was also assessed. Saturation analysis revealed [3H]EBOB binding at a single site, with a K(d) of approximately 9 nM in alpha1beta2gamma2 and alpha2beta2gamma2 receptors. Binding of both [3H]EBOB and [35S]TBPS was inhibited by dieldrin, lindane, tert-butylbicycloorthobenzoate (TBOB), PTX, TBPS, and pentylenetetrazol (PTZ) at one site in a concentration-dependent fashion. Affinities were in the high nM to low microM range for all compounds except PTZ (low mM range), and the rank order of potency for these convulsants to displace [3H]EBOB and [35S]TBPS was the same. Low [GABA] stimulated [3H]EBOB binding, while higher [GABA] (greater than 10 microM) inhibited [3H]EBOB binding. Overall, our data demonstrate that [3H]EBOB binds to a single, high affinity site in alpha1beta2gamma2 and alpha2beta2gamma2 GABAA receptors, and modulation of its binding is similar to that seen with [35S]TBPS. [3H]EBOB has a number of desirable traits that may make it preferable to [35S]TBPS for analysis of the convulsant site of the GABAA receptor.

  3. Role of 2p-2h MEC excitations in superscaling

    Energy Technology Data Exchange (ETDEWEB)

    De Pace, A. E-mail: depace@to.infn.it; Nardi, M.; Alberico, W.M.; Donnelly, T.W.; Molinari, A

    2004-09-06

    Following recent studies of inclusive electron scattering from nuclei at high energies which focused on two-nucleon emission mediated by meson-exchange currents, in this work the superscaling behavior of such contributions is investigated. Comparisons are made with existing data below the quasielastic peak where at high momentum transfers scaling of the second kind is known to be excellent and scaling of the first kind is good, in the proximity of the peak where both 1p-1h and 2p-2h contributions come into play, and above the peak where inelasticity becomes important and one finds scaling violations of the two kinds.

  4. Dehydrocoupling of dimethylamine borane catalyzed by Rh(PCy3)2H2Cl.

    Science.gov (United States)

    Sewell, Laura J; Huertos, Miguel A; Dickinson, Molly E; Weller, Andrew S; Lloyd-Jones, Guy C

    2013-04-15

    The Rh(III) species Rh(PCy3)2H2Cl is an effective catalyst (2 mol %, 298 K) for the dehydrogenation of H3B·NMe2H (0.072 M in 1,2-F2C6H4 solvent) to ultimately afford the dimeric aminoborane [H2BNMe2]2. Mechanistic studies on the early stages in the consumption of H3B·NMe2H, using initial rate and H/D exchange experiments, indicate possible dehydrogenation mechanisms that invoke turnover-limiting N-H activation, which either precedes or follows B-H activation, to form H2B═NMe2, which then dimerizes to give [H2BNMe2]2. An additional detail is that the active catalyst Rh(PCy3)2H2Cl is in rapid equilibrium with an inactive dimeric species, [Rh(PCy3)H2Cl]2. The reaction of Rh(PCy3)2H2Cl with [Rh(PCy3)H2(H2)2][BAr(F)4] forms the halide-bridged adduct [Rh(PCy3)2H2(μ-Cl)H2(PCy3)2Rh][BAr(F)4] (Ar(F) = 3,5-(CF3)2C6H3), which has been crystallographically characterized. This dinuclear cation dissociates on addition of H3B·NMe2H to re-form Rh(PCy3)2H2Cl and generate [Rh(PCy3)2H2(η(2)-H3B·NMe2H)][BAr(F)4]. The fate of the catalyst at low catalyst loadings (0.5 mol %) is also addressed, with the formation of an inactive borohydride species, Rh(PCy3)2H2(η(2)-H2BH2), observed. On addition of H3B·NMe2H to Ir(PCy3)2H2Cl, the Ir congener Ir(PCy3)2H2(η(2)-H2BH2) is formed, with concomitant generation of the salt [H2B(NMe2H)2]Cl.

  5. Synthesis of 3-{4-[4-(Benzylideneaminobenzenesulfonyl]- phenyl}-2-phenylquinazolin-4(3H-one

    Directory of Open Access Journals (Sweden)

    Sunil Manohar Babu

    2009-01-01

    Full Text Available The present work describes the synthesis of a Schiff base, 3-{4-[4-(benzylideneamino benzenesulfonyl]phenyl}-2-phenylquinazolin-4(3H-one from a novel quinazolinone, 3-[4-(4 aminobenzenesulfonylphenyl]-2-phenylquinazolin-4(3H-one. The quinazolinone was prepared by reacting 2-phenyl-4H-3,1 benzoxazin-4-one with dapsone. The structure of the synthesized Schiff base is confirmed by IR, 1H NMR, 13C NMR, MS and elemental analysis.-

  6. Thermodynamic Modeling of the SRS Evaporators: Part II. The 3H System

    Energy Technology Data Exchange (ETDEWEB)

    Jantzen, C.M.

    2001-10-02

    Accumulations of two solid phases have formed scale deposits in the Savannah River Site 2H Evaporator system since late 1996. The aluminosilicate scale deposits caused the evaporator pot to become inoperable in October 1999. Accumulations of the diuranate phase have caused criticality concerns in the SRS 2H Evaporator. In order to ensure that similar deposits are not and will not form in the SRS 3H Evaporator, thermodynamically derived activity diagrams specific to the feeds processed from Tanks 30 and 32 are evaluated in this report.

  7. Uptake of [3H]-nicotine and [3H]-noradrenaline by cultured chromaffin cells.

    Science.gov (United States)

    Ceña, V.; García, A. G.; Montiel, C.; Sánchez-García, P.

    1984-01-01

    Three day-old cultured bovine adrenal chromaffin cells incubated at room temperature with Krebs-HEPES solution containing different concentrations of [3H]-nicotine, took up and retained increasing amounts of the drug by a mechanism that did not saturate. Concentrations of cold nicotine as high as 100 microM did not alter the amount of [3H]-nicotine retained by cells. Imipramine, cocaine, tetracaine or mecamylamine, at concentrations (10 microM) that blocked the catecholamine secretory effects of nicotine completely, did not modify the uptake of [3H]-nicotine. Both imipramine and cocaine drastically inhibited [3H]-noradrenaline uptake by cells in a concentration-dependent manner (IC50S of 0.08 and 1 microM, respectively). These data indicate that the secretory effects of nicotine are not coupled to its previous uptake into cells, and are evidence in favour of a site of action for nicotine located in or at the surface of the chromaffin cell membrane. PMID:6704577

  8. Vicinal 1H-1H NMR coupling constants from density functional theory as reliable tools for stereochemical analysis of highly flexible multichiral center molecules.

    Science.gov (United States)

    López-Vallejo, Fabian; Fragoso-Serrano, Mabel; Suárez-Ortiz, Gloria Alejandra; Hernández-Rojas, Adriana C; Cerda-García-Rojas, Carlos M; Pereda-Miranda, Rogelio

    2011-08-05

    A protocol for stereochemical analysis, based on the systematic comparison between theoretical and experimental vicinal (1)H-(1)H NMR coupling constants, was developed and applied to a series of flexible compounds (1-8) derived from the 6-heptenyl-5,6-dihydro-2H-pyran-2-one framework. The method included a broad conformational search, followed by geometry optimization at the DFT B3LYP/DGDZVP level, calculation of the vibrational frequencies, thermochemical parameters, magnetic shielding tensors, and the total NMR spin-spin coupling constants. Three scaling factors, depending on the carbon atom hybridizations, were found for the (1)H-C-C-(1)H vicinal coupling constants: f((sp3)-(sp3)) = 0.910, f((sp3)-(sp2)) = 0.929, and f((sp2)-(sp2))= 0.977. A remarkable correlation between the theoretical (J(pre)) and experimental (1)H-(1)H NMR (J(exp)) coupling constants for spicigerolide (1), a cytotoxic natural product, and some of its synthetic stereoisomers (2-4) demonstrated the predictive value of this approach for the stereochemical assignment of highly flexible compounds containing multiple chiral centers. The stereochemistry of two natural 6-heptenyl-5,6-dihydro-2H-pyran-2-ones (14 and 15) containing diverse functional groups in the heptenyl side chain was also analyzed by application of this combined theoretical and experimental approach, confirming its reliability. Additionally, a geometrical analysis for the conformations of 1-8 revealed that weak hydrogen bonds substantially guide the conformational behavior of the tetraacyloxy-6-heptenyl-2H-pyran-2-ones.

  9. Characterization of heroin samples by 1H NMR and 2D DOSY 1H NMR.

    Science.gov (United States)

    Balayssac, Stéphane; Retailleau, Emmanuel; Bertrand, Geneviève; Escot, Marie-Pierre; Martino, Robert; Malet-Martino, Myriam; Gilard, Véronique

    2014-01-01

    Twenty-four samples of heroin from different illicit drug seizures were analyzed using proton Nuclear Magnetic Resonance ((1)H NMR) and two-dimensional diffusion-ordered spectroscopy (2D DOSY) (1)H NMR. A careful assignment and quantification of (1)H signals enabled a comprehensive characterization of the substances present in the samples investigated: heroin, its main related impurities (6-acetylmorphine, acetylcodeine, morphine, noscapine and papaverine) and cutting agents (caffeine and acetaminophen in nearly all samples as well as lactose, lidocaine, mannitol, piracetam in one sample only), and hence to establish their spectral signatures. The good agreement between the amounts of heroin, noscapine, caffeine and acetaminophen determined by (1)H NMR and gas chromatography, the reference method in forensic laboratories, demonstrates the validity of the (1)H NMR technique. In this paper, 2D DOSY (1)H NMR offers a new approach for a whole characterization of the various components of these complex mixtures.

  10. Differential binding of /sup 3/H-imipramine and /sup 3/H-mianserin in rat cerebral cortex

    Energy Technology Data Exchange (ETDEWEB)

    Dumbrille-Ross, A.; Tang, S.W.; Coscina, D.V.

    1981-11-16

    Drug competition profiles, effect of raphe lesion, and sodium dependency of the binding of two antidepressant drugs /sup 3/H-imipramine and /sup 3/H-mianserin to rat cerebral cortex homogenate were compared to examine whether the drugs bound to a common ''antidepressant receptor.'' Of the neurotransmitters tested, only serotonin displaced binding of both /sup 3/H-imipramine and /sup 3/H-mianserin. /sup 3/H-Mianserin binding was potently displaced by serotonin S/sub 2/ antagonists and exhibited a profile similar to that of /sup 3/H-spiperone binding. In the presence of the serotonin S/sub 2/ antagonist spiperone, antihistamines (H/sub 1/) potently displaced /sup 3/H-mianserin binding. /sup 3/H-Imipramine binding was displaced potently by serotonin uptake inhibitors. The order of potency of serotonergic drugs in displacing /sup 3/H-imipramine binding was not similar to their order in displacing /sup 3/H-spiperone or -3H-serotonin binding. Prior midbrain raphe lesions greatly decreased the binding of /sup 3/H-imipramine but did not alter binding of /sup 3/H-mianserin. Binding of /sup 3/H-imipramine but not /sup 3/H-mianserin was sodium dependent. These results show that /sup 3/H-imipramine and /sup 3/H-mianserin bind to different receptors. /sup 3/H-Imipramine binds to a presynaptic serotonin receptor which is probably related to a serotonin uptake recognition site, the binding of which is sodium dependent. /sup 3/H-Mianserin binds to postsynaptic receptors, possibly both serotonin S/sub 2/ and histamine H/sub 1/ receptors, the binding of which is sodium independent.

  11. 一类2(1H)-喹喔啉衍生物的紫外光谱研究%Study on the Ultraviolet Spectrum in a Series of 2(1H)-Quinoxalin-2-one Derivatives

    Institute of Scientific and Technical Information of China (English)

    杨小兵; 丁松涛; 王安邦; 杨裕生

    2003-01-01

    研究了一类喹喔啉衍生物,1-烷基-3-甲基-2(1H)-喹喔啉-2-酮(1-alkyl-3-methyl-2(1H)-quinoxalin-2-one,简称AMQ, 其中alkyl =H, CH3, C2H5,n-C3H7,n-C5H11,n-C16H33)的紫外吸收光谱.这类化合物可应用于药物,如用作α-氨基羟甲基异恶唑丙酸(AMPA)受体拮抗剂、杀菌剂等;还可用作植物生长调节剂、荧光探针等领域.结果表明:化合物中氮原子上烷基链的增长对该类喹喔啉衍生物的紫外吸收光谱基本没有影响,谱图中峰形大体相同.紫外吸收谱图中,在327和340 nm左右有两个吸收强度相当的一对肩峰,280 nm处有一个吸收强度稍弱的峰;340 nm左右的吸收峰主要是n→Π*跃迁所致,其中也含有Π→Π*跃迁的成分;327和280 nm左右强吸收峰是Π→Π*跃迁所致.

  12. Intense laser induced field ionization of C2H2, C2H4,and C2H6

    Institute of Scientific and Technical Information of China (English)

    GAO Lirong; JI Na; XONG Yijia; TANG Xiaoping; KONG Fan'ao

    2003-01-01

    Using HOMO Field Ionization Model, the tunneling probabilities and the theoretical threshold intensities of the field ionizations of acetylene, ethylene, and ethane in intense laser field are calculated. C2H2, C2H4, and C2H6 were irradiated by 800 nm, 100 fs laser pulses with the intensity range of 1013-1014 W/cm2. A TOF-mass spectrometer was coupled to the laser system and used to experimentally investigate the field ionization of these molecules. The experimental ionization threshold intensities are obtained. The calculating results of the three molecules agree well with the experimental results, indicating that HOMO Field Ionization Model is valid for the ionization of polyatomic molecules in intense laser field.

  13. One-step preparation of [2,3-{sup 3}H]1-aminocyclo-propanecarboxylic acid: a useful ligand for strychnine-insensitive glycine receptors

    Energy Technology Data Exchange (ETDEWEB)

    Lewin, A.H.; Lamb, P.B. [Research Triangle Inst., Research Triangle Park, NC (United States); Popik, P.; Skolnick, P. [National Insts. of Health, Bethesda, MD (United States)

    1994-11-01

    Catalytic hydrogenation of 1-aminocyclopropenecarboxylic acid under tritium gas afforded [2,3-{sup 3}H]1-aminocyclopropanecarboxylic acid with specific activity 26 Ci/mmol, determined by a combination of {sup 1}H and {sup 3}H NMR. Pilot radioligand binding assays indicate this compound will be a useful prove for the NMDA receptor-associated strychnine-insensitive glycine receptor. (author).

  14. Anomalous Absorption in Cyclic C$_3$H Radical

    CERN Document Server

    Chandra, S; Chandra, Suresh

    2003-01-01

    Yamamoto et al. (1987) reported the first detection of $c$-C$_3$H radical in {TMC-1} through its transition $2_{1 2} \\to 1_{1 1}$ at 91.5 GHz. Mangum and Wootten (1990) detected $c$-C$_3$H through the transition $1_{1 0} \\to 1_{1 1}$ at 14.8 GHz in 12 additional galactic objects. The column density of $c$-C$_3$H in the objects was estimated to be about one order of magnitude lower than that of the C$_3$H$_2$ which is ubiquitous in the galactic objects. The most probable production mechanism of both the C$_3$H and C$_3$H$_2$ in dark clouds is a common dissociation reaction of C$_3$H$_3^+$ ion (Adams & Smith, 1987). Although the $c$-C$_3$H is 0.8 eV less stable than its isomer $l$-C$_3$H, finding of comparable column densities of both the isomers in {TMC-1} supports the idea of comparable formation of both the $c$-C$_3$H and $l$-C$_3$H in the cosmic objects. Existence of a metaisomer in interstellar condition is a well known phenomenon in astronomy. We propose that $c$-C$_3$H may be identified through the t...

  15. THz spectroscopy of D2H+

    Science.gov (United States)

    Yu, S.; Pearson, J. C.; Amano, T.; Matsushima, F.

    2017-01-01

    We extended the measurements of the rotational transitions of D2H+ up to 3 THz by using the JPL frequency multiplier chains and a TuFIR system at Toyama. D2H+ was generated in an extended negative glow discharge cell cooled to liquid nitrogen temperature. We observed five new THz lines. All the available rotational transition frequencies together with the combination differences derived from the three fundamental bands were subject to least square analysis to determine the molecular constants. New THz measurements are definitely useful for better characterization of spectroscopic properties. The improved molecular constants provide better predictions of other unobserved rotational transitions.

  16. Depolarization-induced release of [(3)H]D-aspartate from GABAergic neurons caused by reversal of glutamate transporters

    DEFF Research Database (Denmark)

    Jensen, J B; Pickering, D S; Schousboe, A;

    2000-01-01

    was blocked by 6-chloro-3,4-dihydro-3-(2-norbornen-5-yl)-2H-1,2, 4-benzothiadiazine-7-sulphonamide-1,1-dioxide (cyclothiazide). Under the non-desensitizing conditions, the AMPA-induced release of [(3)H]D-aspartate was highly enhanced showing about a 10-fold increase over basal release. Addition of cobalt...

  17. HIV-1 Vif adaptation to human APOBEC3H haplotypes.

    Science.gov (United States)

    Ooms, Marcel; Brayton, Bonnie; Letko, Michael; Maio, Susan M; Pilcher, Christopher D; Hecht, Frederick M; Barbour, Jason D; Simon, Viviana

    2013-10-16

    Several human APOBEC3 deaminases can inhibit HIV-1 replication in vitro. HIV-1 Vif counteracts this restriction by targeting APOBEC3 for proteasomal degradation. Human APOBEC3H (A3H) is highly polymorphic, with natural variants differing considerably in anti-HIV-1 activity in vitro. To examine HIV-1 adaptation to variation in A3H activity in a natural infection context, we determined the A3H haplotypes and Vif sequences from 76 recently infected HIV-1 patients. We detected A3H-specific Vif changes suggesting viral adaptation. The patient-derived Vif sequences were used to engineer viruses that specifically differed in their ability to counteract A3H. Replication of these Vif-variant viruses in primary T cells naturally expressing active or inactive A3H haplotypes showed that endogenously expressed A3H restricts HIV-1 replication. Proviral DNA from A3H-restricted viruses showed high levels of G-to-A mutations in an A3H-specific GA dinucleotide context. Taken together, our data validate A3H expressed at endogenous levels as a bona fide HIV-1 restriction factor.

  18. An iron(III) complex salt containing pyrazole as both ligand and counter-ion: bis(1H-pyrazol-2-ium) pentacyanido(1H-pyrazole-κN(2))ferrate(III).

    Science.gov (United States)

    Wang, Yu-Feng; Yu, Chun-Hua; Zhu, Run-Qiang

    2014-05-01

    The title compound, (C3H5N2)2[Fe(CN)5(C3H4N2)], is composed of a mononuclear [Fe(CN)5(pyrazole)](2-) dianion and two 1H-pyrazol-2-ium cations. A three-dimensional supramolecular network is formed through a rich scheme of N-H...N hydrogen bonds and C-H...π interactions among the cations and anions.

  19. Metabolism of orally administered (/sup 3/H)ergocalciferol and (/sup 3/H)cholecalciferol by dairy calves

    Energy Technology Data Exchange (ETDEWEB)

    Sommerfeldt, J.L.; Napoli, J.L.; Littledike, E.T.; Beitz, D.C.; Horst, R.L.

    1983-12-01

    Concentrations of ergocalciferol, cholecalciferol, and their metabolites in plasma were determined after a single oral dose of (/sup 3/H)ergocalciferol or (/sup 3/H)cholecalciferol was given to 95- to 105-kg Jersey bull calves. One group (three calves) was given 365 muCi of (/sup 3/H)ergocalciferol (1.2 Ci/mmol) per calf, and the other group (three calves) was given 365 muCi of (/sup 3/H)cholecalciferol (1.2 Ci/mmol) per calf. Fourteen blood samples were taken from each calf during the 3 weeks after administration. Total plasma radioactivity was highest at 80 hours in both groups (8400 dpm/ml and 4600 dpm/ml in the (/sup 3/H)cholecalciferol- and (/sup 3/H)ergocalciferol-treated calves, respectively). For determination of the time-dependent appearance and disappearance of plasma vitamin D and vitamin D metabolites, the plasma /sup 3/H-labeled steroids were extracted and separated by high-performance liquid chromatography. In both groups, (/sup 3/H)vitamin D peaked at 24-48 hours and was the predominant radioactive form in plasma 10-15 hours after dosing. After 15 hours, 25-(/sup 3/H)hydroxyvitamin D became the predominant labeled metabolite, reaching its maximal concentration between 48 and 96 hours. Concentrations of 25-(/sup 3/H)hydroxycholecalciferol were about twice those of 25-(/sup 3/H)hydroxyergocalciferol. The appearance/disappearance profile of 25,26-(/sup 3/H)dihydroxycholecalciferol and 1,25(/sup 3/H)hydroxycholecalciferol resembled that of 25-(/sup 3/H)hydroxycholecalciferol.

  20. Expeditious diastereoselective synthesis of elaborated ketones via remote Csp3-H functionalization

    Science.gov (United States)

    Shu, Wei; Lorente, Adriana; Gómez-Bengoa, Enrique; Nevado, Cristina

    2017-01-01

    The quest for selective C-H functionalization reactions, able to provide new strategic opportunities for the rapid assembly of molecular complexity, represents a major focus of the chemical community. Examples of non-directed, remote Csp3-H activation to forge complex carbon frameworks remain scarce due to the kinetic stability and thus intrinsic challenge associated to the chemo-, regio- and stereoselective functionalization of aliphatic C-H bonds. Here we describe a radical-mediated, directing-group-free regioselective 1,5-hydrogen transfer of unactivated Csp3-H bonds followed by a second Csp2-H functionalization to produce, with exquisite stereoselectivity, a variety of elaborated fused ketones. This study demonstrates that aliphatic acids can be strategically harnessed as 1,2-diradical synthons and that secondary aliphatic C-H bonds can be engaged in stereoselective C-C bond-forming reactions, highlighting the potential of this protocol for target-oriented natural product and pharmaceutical synthesis.

  1. Partial chemical characterization of cyclopyrrolones ((/sup 3/H) suriclone) and benzodiazepines ((/sup 3/H)flunitrazepam) binding site: Differences

    Energy Technology Data Exchange (ETDEWEB)

    Zundel, J.L.; Blanchard, J.C.; Julou, L.

    1985-06-10

    Rat hippocampus membranes were treated with several protein modifying reagents (iodoacetamide, N-ethylmaleimide, tetranitromethane and N-acetylimidazole). The effects of these treatments on the binding sites of cyclopyrrolones ((/sup 3/H) suriclone), a new chemical family of minor tranquilizers, and benzodiazepines ((/sup 3/H) flunitrazepam) were investigated. Here the authors show that both ligands are similarly sensitive to cysteine alkylation: (/sup 3/H) suriclone and (/sup 3/H) flunitrazepam binding are reduced by iodoacetamide and slightly increased by N-ethylmaleimide. On the contrary they are clearly differentiated by tyrosine modification: (/sup 3/H) suriclone binding is not changed whereas (/sup 3/H) flunitrazepam binding is increased by tetranitromethane and decreased by N-acetylimidazole. The present findings and published evidence suggest cyclopyrrolones and benzodiazepines bind to distinct sites or to different allosteric forms of the benzodiazepine receptor. 28 references, 6 figures.

  2. Main: 1V3H [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1V3H 大豆 Soybean Glycine max (L.) Merrill Beta-Amylase Name=Bmy1; Glycine Max Molecule: Beta-Amylase; Chai... 495 AA, Molecular weight: 56011 Da ATSDSNMLLNYVPVYVMLPLGVVNVDNVFEDPDGLKEQLLQLRAAGVDGVMVDVWWGIIELKGPKQYDWRAYRSLFQLVQECGLTLQAI...MSFHQCGGNVGDIVNIPIPQWVLDIGESNHDIFYTNRSGTRNKEYLTVGVDNEPIFHGRTAIEIYSDYMKSFRENMSDFLESGLIIDIEVG...FLTWYSNKLLNHGDQILDEANKAFLGCKVKLAIKVSGIHWWYKVENHAAELTAGYYNLNDRDGYRPIARMLSRHHAILNFTCLEMRDSEQPSDAKSGPQELVQQVLSG...GWREDIRVAGENALPRYDATAYNQIILNAKPQGVNNNGPPKLSMFGVTYLRLSDDLLQKSNFNIFKKFVLKMHADQDYCANPQKYNHAITPLKPSAPKIPIEVLLEATKPTLPFPWLPETDMKVDG soybean_1V3H.jpg ...

  3. catena-Poly[[(diiodidocadmium-μ-{1-[(1H-benzimidazol-2-ylmethyl]-1H-imidazole-κ2N:N′}] N,N-dimethylformamide monosolvate

    Directory of Open Access Journals (Sweden)

    Bingtao Liu

    2011-12-01

    Full Text Available In the title complex, {[CdI2(C11H10N4]·C3H7NO}n, the CdII ion is four-coordinated by two N atoms from two 1-[(1H-benzimidazol-1-ylmethyl]-1H-imidazole (bmi ligands and by two terminal I− anions in a distorted tetrahedral geometry. One of the two I− anions is disordered over two sets of sites, with refined occupancies of 0.66 (5 and 0.34 (5. The CdII ions are bridged by bmi ligands, leading to the formation of a chain along [001]. Dimethylformamide solvent molecules are located between these chains. Classical N—H...O hydrogen bonding between the bmi ligands and the solvent molecules leads to a consolidation of the structure.

  4. Group theoretical analysis of the H3+ +H2 ↔ H5+ reaction

    Science.gov (United States)

    Lin, Zhou

    2016-06-01

    The H3+ +H2 →H2 + H3+ proton transfer reaction is complicated due to the proton scrambling from the large amplitude motions in the H5+ intermediate. In order to understand this reaction, high-resolution spectroscopic studies are necessary for the reactants/products and the intermediate, and the group theoretical analysis is an essential aspect in the prediction and interpretation of these spectra. With five indistinguishable protons, H5+ is characterized using the G240 complete nuclear permutation-inversion (CNPI) group. For most of the configurations sampled by the reaction path, the feasible permutations depend on the distance between the H3+ and H2 fragments. Subgroups of G240 can be used to describe these feasible permutations. Specifically, we consider two limits of the molecular configurations. The equilibrium structure of H5+ , i.e., [H2 -H -H2 ]+, can be described using the G16 molecular symmetry group, while the dissociation products, i.e., H3+ ⋯H2 , require the G24 molecular symmetry group. In the present study, a group theoretical analysis is performed for both limits, providing the symmetries for the nuclear spins and rovibrational wave functions. Also, spectroscopic properties for [H2 -H -H2 ]+, particularly rovibrational couplings and electric dipole selection rules, as well as correlations of energy levels between [H2 -H -H2 ]+ and H3+ ⋯H2 , are obtained.

  5. Thermolysis and solid state NMR studies of NaB3H8, NH3B3H7, and NH4B3H8.

    Science.gov (United States)

    Huang, Zhenguo; Eagles, Mitch; Porter, Spencer; Sorte, Eric G; Billet, Beau; Corey, Robert L; Conradi, Mark S; Zhao, Ji-Cheng

    2013-01-21

    In an effort to broaden the search for high-capacity hydrogen storage materials, three triborane compounds, NaB(3)H(8), NH(3)B(3)H(7), and NH(4)B(3)H(8), were studied. In addition to hydrogen, thermal decomposition also releases volatile boranes, and the relative amounts and species depend on the cations (Na(+), NH(4)(+)) and the Lewis base (NH(3)). Static-sample hydrogen NMR is used to probe molecular motion in the three solids. In each case, the line width decreases from low temperatures to room temperature in accordance with a model of isotropic or nearly isotropic reorientations. Such motions also explain a deep minimum in the relaxation time T(1). Translational diffusion never appears to be rapid on the 10(-5) s time scale of NMR.

  6. Palladium(0)-Catalyzed Benzylic C(sp(3))-H Functionalization for the Concise Synthesis of Heterocycles and Its Applications.

    Science.gov (United States)

    Tsukano, Chihiro

    2017-01-01

    C-H functionalization reactions involve the activation of otherwise unreactive C-H bonds, and represent atom economical methods for the direct transformation of simple substrates to complex molecules. While transition metal-catalyzed C(sp(2))-H functionalization reactions are regularly used in synthesis, C(sp(3))-H functionalization is rarely applied to the synthesis of complex natural products because of the difficulties associated with controlling selectivity. With this in mind, we focused on the development of new palladium (Pd)(0)-catalyzed C(sp(3))-H functionalization reactions for the synthesis of complex molecules, resulting in several new methods capable of solving these problems. We initially developed a concise synthetic method for the facile construction of oxindoles and spirooxindoles via a Pd-catalyzed benzylic C(sp(3))-H functionalization reaction. This method was subsequently extended to the synthesis of various heterocycles, including 2-arylindoles, benzocarbazole, indolocarbazole, indoloquinazolinone, and indoloquinazolinedione, as well as the total synthesis of several pyrrolophenanthridine alkaloids without the need for any protecting groups. This method was also successfully applied to the synthesis of the right-hand fragment of benzohopane from tetrahydro-2H-fluorene, which was constructed by a Pd-catalyzed benzylic C(sp(3))-H functionalization. In this review, we provide a detailed discussion of our most recent investigations pertaining to Pd(0)-catalyzed benzylic C(sp(3))-H functionalization.

  7. Localization of [3H]nicotine, [3H]cytisine, [3H]epibatidine, and [125I]alpha-bungarotoxin binding sites in the brain of Macaca mulatta.

    Science.gov (United States)

    Han, Zhi-Yan; Zoli, Michele; Cardona, Ana; Bourgeois, Jean-Pierre; Changeux, Jean-Pierre; Le Novère, Nicolas

    2003-06-16

    We determined the localization of [(3)H]nicotine, [(3)H]cytisine, [(3)H]epibatidine, and [(125)I]alpha-bungarotoxin binding sites in the brain of rhesus monkey by means of receptor autoradiography. The labelings by [(3)H]nicotine, [(3)H]cytisine, and [(3)H]epibatidine were highly concordant, except for epibatidine. Layer IV of some cortical areas, most thalamic nuclei, and presubiculum displayed high levels of labeling for the three ligands. Moderate levels of binding were detected in the subiculum, the septum, and the mesencephalon. Low levels were present in layers I-II and VI of the cortex, the cornu Ammonis, the dentate gyrus, and the amygdala. In addition, the level of epibatidine labeling was very high in the epithalamic nuclei and the interpeduncular nucleus, whereas labeling by nicotine and cytisine was very weak in the same regions. The distribution of [(125)I]alpha-bungarotoxin binding differed from the binding of the three agonists. The labeling was dense in layer I of most cortical areas, dentate gyrus, stratum lacunosum-moleculare of CA1 field, several thalamic nuclei, and medial habenula. A moderate labeling was found in layers V and VI of the prefrontal and frontal cortices, layer IV of primary visual cortex, amygdala, septum, hypothalamus, and some mesencenphalic nuclei. A weak signal was also detected in subiculum, claustrum, stratum oriens, and stratum lucidum of cornu Ammonis and also in some mesencephalic nuclei. The distribution of nicotine, cytisine, and epibatidine bindings corresponds broadly to the patterns observed in rodents, with the marked exception of the epithalamus. However, in monkey, those distributions match the distribution of alpha2 messenger RNA, rather than that of alpha4 transcripts as it exists in rodent brains. The distribution of the binding sites for alpha-bungarotoxin is larger in the brain of rhesus monkeys than in rodent brain, suggesting a more important role of alpha7 receptors in primates.

  8. CCQE, 2p2h excitations and \

    CERN Document Server

    Nieves, J; Sánchez, F; Vacas, M J Vicente

    2013-01-01

    We analyze the MiniBooNE muon neutrino CCQE-like d\\sigma/dT_\\mu/dcos\\theta_\\mu data using a theoretical model that, among other nuclear effects, includes RPA correlations and 2p2h (multinucleon) mechanisms. These corrections turn out to be essential for the description of the data. We find that MiniBooNE CCQE-like data are fully compatible with former determinations of the nucleon axial mass M_A ~ 1.05 GeV. This is in sharp contrast with several previous analysis where anomalously large values of M_A ~ 1.4 GeV have been suggested. We also show that because of the the multinucleon mechanism effects, the algorithm used to reconstruct the neutrino energy is not adequate when dealing with quasielastic-like events. Finally, we analyze the MiniBooNE unfolded cross section, and show that it exhibits an excess (deficit) of low (high) energy neutrinos, which is an artifact of the unfolding process that ignores 2p2h mechanisms.

  9. Observation of 1H-13C and 1H-1H proximities in a paramagnetic solid by NMR at high magnetic field under ultra-fast MAS

    Science.gov (United States)

    Li, Shenhui; Trébosc, Julien; Lafon, Olivier; Zhou, Lei; Shen, Ming; Pourpoint, Frédérique; Amoureux, Jean-Paul; Deng, Feng

    2015-02-01

    The assignment of NMR signals in paramagnetic solids is often challenging since: (i) the large paramagnetic shifts often mask the diamagnetic shifts specific to the local chemical environment, and (ii) the hyperfine interactions with unpaired electrons broaden the NMR spectra and decrease the coherence lifetime, thus reducing the efficiency of usual homo- and hetero-nuclear NMR correlation experiments. Here we show that the assignment of 1H and 13C signals in isotopically unmodified paramagnetic compounds with moderate hyperfine interactions can be facilitated by the use of two two-dimensional (2D) experiments: (i) 1H-13C correlations with 1H detection and (ii) 1H-1H double-quantum ↔ single-quantum correlations. These methods are experimentally demonstrated on isotopically unmodified copper (II) complex of L-alanine at high magnetic field (18.8 T) and ultra-fast Magic Angle Spinning (MAS) frequency of 62.5 kHz. Compared to 13C detection, we show that 1H detection leads to a 3-fold enhancement in sensitivity for 1H-13C 2D correlation experiments. By combining 1H-13C and 1H-1H 2D correlation experiments with the analysis of 13C longitudinal relaxation times, we have been able to assign the 1H and 13C signals of each L-alanine ligand.

  10. Synthesis and antimicrobial activities of new oxime carbamates of 3-aryl-2-thioquinazolin-4(3H)-one

    Indian Academy of Sciences (India)

    Suresh S Patil; Swati D Jadhav; M B Deshmukh

    2012-09-01

    S-alkylation of 3-aryl-2-thioquinazolin-4(3H)-one (1) with chloroacetone gave 2-(propanonyl thio)-3-arylquinazol-4(3H)ones (2). Further, the treatment of compound (2) with hydroxylamine hydrochloride gave the corresponding oximes (3) which on reaction with phenyl isocyanate in THF yielded corresponding oxime carbamates 4. The synthesized compounds have been confirmed using IR and 1H NMR, mass spectral data together with elemental analysis. All newly synthesized compounds have been tested for their antibacterial and antifungal activities.

  11. Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole}sulfatozinc(II dihydrate

    Directory of Open Access Journals (Sweden)

    Yan-Zhi Wang

    2010-11-01

    Full Text Available In the title complex, [Zn(SO4(C9H8N6(H2O4]·2H2O, the ZnII ion is six-coordinated by one N atom from a 1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole ligand and five O atoms from one monodentate sulfate anion and four water molecules in a distorted octahedral geometry. The sulfate tetrahedron is rotationally disordered over two positions in a 0.618 (19:0.382 (19 ratio. In the crystal, adjacent molecules are linked through O—H...O and O—H...N hydrogen bonds involving the cation, the anion, and the coordinated and uncoordinated water molecules into a three-dimensional network.

  12. Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole}sulfatocadmium dihydrate

    Directory of Open Access Journals (Sweden)

    Yu-xian Li

    2011-09-01

    Full Text Available In the title complex, [Cd(SO4(C9H8N6(H2O4]·2H2O, the CdII ion is six-coordinated by one N atom from a 1-[(1H-1,2,3-benzotriazol-1-ylmethyl]-1H-1,2,4-triazole ligand and by five O atoms from four water molecules and one monodentate sulfate anion in a distorted octahedral geometry. The sulfate tetrahedron is rotationally disordered over two positions in a 0.651 (12:0.349 (12 ratio. In the crystal, adjacent molecules are linked through O—H...O and O—H...N hydrogen bonds into a three-dimensional network.

  13. Synthesis and Molecular Structure of 1,5,1',5'-Tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazole

    Institute of Scientific and Technical Information of China (English)

    JIANG Wen-Qing; LIU Tian-Bao; ZOU Jian-Ping; ZHANG Yong

    2007-01-01

    The title compound 1,5,1',5'-tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazole (2, C28H20N6S2, Mr=504.62) was prepared by the reaction of 1-benzoyl-3-phenylaminothiourea 1 and Mn(OAc)3·2H2O in acetic acid under microwave irradiation. The crystal is of monoclinic, space group P21/c with a=11.3931(10), b=16.5787(14), c=26.470(2) (A), β=98.274(2)°, Z=8, V=4947.8(8) (A)3, Dc=1.355 g/cm3, μ(MoKα) (A) 0.245 mm-1, F(000)=2096, the final R=0.0583 and Wr=0.1502 for 8705 observed reflections (Ⅰ > 2σ(Ⅰ)). X-ray analysis reveals that the title compound is 1,5,1',5'-tetraphenyl-1H,1H'-3,3'-dialkylthio-bi-1,2,4-triazole, and its formation mechanism was proposed.

  14. Crystalline 1H-1,2,3-triazol-5-ylidenes

    Energy Technology Data Exchange (ETDEWEB)

    Bertrand, Guy; Gulsado-Barrios, Gregorio; Bouffard, Jean; Donnadieu, Bruno

    2016-08-02

    The present invention provides novel and stable crystalline 1H-1,2,3 triazolium carbenes and metal complexes of 1H-1,2,3 triazolium carbenes. The present invention also provides methods of making 1H-1,2,3 triazolium carbenes and metal complexes of 1H-1,2,3 triazolium carbenes. The present invention also provides methods of using 1H-1,2,3 triazolium carbenes and metal complexes of 1H-1,2,3 triazolium carbenes in catalytic reactions.

  15. KBS-3H Complementary studies, 2008-2010

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2012-10-15

    KBS-3H is a joint project between Svensk Kaernbraenslehantering AB (SKB) in Sweden and Posiva Oy in Finland. The main goal during the project phase Complementary studies of horizontal emplacement KBS-3H 2008-2010 was to develop KBS-3H to such a state that a decision to go ahead with full-scale testing and demonstration could be made. The KBS-3H design is a variant of the KBS-3 method and an alternative to the KBS-3V design. In KBS-3H multiple canisters containing spent nuclear fuel are emplaced in parallel, 100-300 m long, horizontal deposition drifts at a depth of about 400-500 m in the bedrock whereas the KBS-3V design calls for vertical emplacement of the canisters in individual deposition holes. Further development and evaluation of the main KBS-3H design alternatives developed in earlier work, DAWE (Drainage, Artificial Watering and air Evacuation) and STC (Semi Tight Compartments) (Autio el al. 2007) has now enabled a well-founded KBS-3H reference design selection, DAWE has been selected. Regarding long-term safety; bentonite-metal interactions have been in focus and studies have given a good basis for material selection for the Supercontainer, plugs and other supporting structures and titanium is selected. The selections and evaluations made during this project phase will be used in the safety evaluations planned for Forsmark and Olkiluoto in the upcoming project phase. KBS-3H specific production lines have been outlined and layout adaptations for both Forsmark and Olkiluoto have been developed. Full-scale tests of system components have also been carried out with good results; the full-scale compartment plug test shows the ability to install a plug that separates drift compartments hydraulically.

  16. Enantiospecific synthesis of (1- sup 3 H)-(+)-pseudoephedrine hydrochloride

    Energy Technology Data Exchange (ETDEWEB)

    Hill, J.A.; Scharver, J.D. (Burroughs Wellcome Co., Research Triangle Park, North Carolina (USA). Chemical Development Labs.)

    1990-06-01

    The naturally occurring dextrorotary enantiomer (+)-pseudoephedrine was synthesized in the ({sup 3}H)-labelled form with specific activity 17.5 Ci/mmol suitable for development of a radioimmunoassay procedure. The chirally specific route from L-alanine to (1-{sup 3}H)-d-pseudoephedrine hydrochloride was based on the use of {alpha}-amino acids as chiral educts for asymmetric products. (author).

  17. Characterization of the 1H-cyclopentapyrimidine-2,4(1H,3H)-dione derivative (S)-CPW399 as a novel, potent, and subtype-selective AMPA receptor full agonist with partial desensitization properties

    DEFF Research Database (Denmark)

    Campiani, G; Morelli, E; Nacci, V

    2001-01-01

    (S)-CPW399 (2b) is a novel, potent, and subtype-selective AMPA receptor full agonist that, unlike (S)-willardiine and related compounds, in mouse cerebellar granule cells, stimulated an increase in [Ca(2+)](i), and induced neuronal cell death in a time- and concentration-dependent manner. Compoun...... 2b appears to be a weakly desensitizing, full agonist at AMPA receptors and therefore represents a new pharmacological tool to investigate the role of AMPA receptors in excitotoxicity and their molecular mechanisms of desensitization....

  18. Optical and electrochemical dual channel sensing of Cu2 + using functionalized furo[2,3-d]pyrimidines-2,4[1H,3H]-diones

    Science.gov (United States)

    Kumar, Manoj; Kumawat, Lokesh Kumar; Bhatt, Priyanka; Jha, Anjali; Agarwal, Shilpi; Sharma, Anuj; Gupta, Vinod Kumar

    2017-06-01

    Owing to their easy accessibility and high degree of structural and functional diversity, many multicomponent reactions (MCRs) have been a rich source of conjugate π-systems, functionalised chromophores (or fluorophore) and redox active molecules. Despite their high explorative potential and practical benefits, only a few MCR products have been so far investigated for their metal sensing abilities. In the present report, two furopyrimidinones (FPys) based molecular systems have been synthesized by [4 + 1] cycloaddition based MCR sequence. Designed chemosensors displayed optic (absorption spectra) as well as electroanalytical (ion selective electrode) response toward Cu2 + ion in solution and membrane phase respectively (dual channel sensing). Different aspects of both the sensing phenomena such as selectivity, association constants, detection limit, membrane composition etc. were studied in detail using UV-Vis spectroscopy, NMR titration and cell assembly. Both the compounds showed excellent performance characteristics such as high selectivity, acceptable affinity and low detection limits (10- 7 M) in both sensing assays with potential utility in the area of sample monitoring.

  19. Discovery of (E)-5-(benzylideneamino)-1H-benzo[d]imidazol-2(3H)-one derivatives as inhibitors for PTK6.

    Science.gov (United States)

    Shim, Hyun Jae; Yang, Hye Ran; Kim, Han Ie; Kang, Shin-Ae; No, Kyoung Tai; Jung, Young Hoon; Lee, Seung-Taek

    2014-10-01

    A lead compound 1, which inhibits the catalytic activity of PTK6, was selected from a chemical library. Derivatives of compound 1 were synthesized and analyzed for inhibitory activity against PTK6 in vitro and at the cellular level. Selected compounds were analyzed for cytotoxicity in human foreskin fibroblasts using MTT assays and for selectivity towards PTK members in HEK 293 cells. Compounds 20 (in vitro IC50=0.12μM) and 21 (in vitro IC50=0.52μM) showed little cytotoxicity, excellent inhibition of PTK6 in vitro and at the cellular level, and selectivity for PTK6. Compounds 20 and 21 inhibited phosphorylation of specific PTK6 substrates in HEK293 cells. Thus, we have identified novel PTK6 inhibitors that may be used as treatments for PTK6-positive carcinomas, including breast cancer. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Crystal structure of (3E)-5-nitro-3-(2-phenyl-hydrazinyl-idene)-1H-indol-2(3H)-one.

    Science.gov (United States)

    Velasques, Jecika Maciel; Gervini, Vanessa Carratu; Bortoluzzi, Adaílton João; de Farias, Renan Lira; de Oliveira, Adriano Bof

    2017-02-01

    The reaction between 5-nitro-isatin and phenyl-hydrazine in acidic ethanol yields the title compound, C14H10N4O3, whose mol-ecular structure deviates slightly from a planar geometry (r.m.s. deviation = 0.065 Å for the mean plane through all non-H atoms). An intra-molecular N-H⋯O hydrogen bond is present, forming a ring of graph-set motif S(6). In the crystal, mol-ecules are linked by N-H⋯O and C-H⋯O hydrogen-bonding inter-actions into a two-dimensional network along (120), and rings of graph-set motif R2(2)(8), R2(2)(26) and R4(4)(32) are observed. Additionally, a Hirshfeld surface analysis suggests that the mol-ecules are stacked along [100] through C=O⋯Cg inter-actions and indicates that the most important contributions for the crystal structure are O⋯H (28.5%) and H⋯H (26.7%) inter-actions. An in silico evaluation of the title compound with the DHFR enzyme (di-hydro-folate reductase) was performed. The isatin-hydrazone derivative and the active site of the selected enzyme show N-H⋯O(ASP29), N-H⋯O(ILE96) and Cg⋯Cg(PHE33) inter-actions.

  1. Crystal structure of 5,5-bis(4-methylbenzylpyrimidine-2,4,6(1H,3H,5H-trione monohydrate

    Directory of Open Access Journals (Sweden)

    Bhaskarachar Ravi Kiran

    2015-01-01

    Full Text Available The asymmetric unit of the title compound, C20H20N2O3·H2O, contains two independent molecules (A and B, with similar conformations and two independent water molecules. In the crystal, N—H...O and Owater—H...O hydrogen bonds link all moieties into two crystallographically independent kinds of sheets parallel to the ac plane. These independent sheets, each containing either A or B molecules, are further alternately stacked along the b axis and interconnected via C—H...πaryl interactions.

  2. Dibromidobis[1-(2-bromobenzyl-3-(pyrimidin-2-yl-1H-imidazol-2(3H-one]copper(II

    Directory of Open Access Journals (Sweden)

    Chun-Xin Lu

    2012-06-01

    Full Text Available In the title complex, [CuBr2(C14H11BrN4O2], the CuII ion is located on an inversion centre and is coordinated by two ketonic O atoms, two N atoms and two Br atoms, forming a distorted octahedral coordination environment. The two carbonyl groups are trans positioned with C=O bond lengths of 1.256 (5 Å, in agreement with a classical carbonyl bond. The Cu—O bond length is 2.011 (3 Å. The two bromobenzyl rings are approximately parallel to one another, forming a dihedral angle of 70.1 (4° with the coordination plane.

  3. Poly[[2-(3-pyridinio-1H,3H+-benzimidazolium] [μ4-oxido-di-μ3-oxido-tetra-μ2-oxido-hexaoxidotetramolybdenum(VI

    Directory of Open Access Journals (Sweden)

    Xiao-Hua Chen

    2009-05-01

    Full Text Available The reaction of MoO3 with 2-(3-pyridylbenzoimidazole and water in the presence of MnSO4·5H2O at 453 K under hydrothermal conditions afforded the title compound, {(C12H11N2[Mo4O13]}n, in which infinite molybdenum oxide anionic chains are charge-balanced by diprotonated 2-(3-pyridylbenzoimidazole (H23-PBIM2+ cations. Eight [MoO6] octahedra are edge-shared, forming compact octamolybdate subunits which are connected through pairs of Mo—O—Mo bridges into extended one-dimensional arrays propagating along the a-axis direction. The asymmetric unit of the metal oxide chain contains one half of the octamolybdate unit, denoted [Mo4O13], the other half being generated by an inversion center. These molybdenum oxide chains are further connected through the 2-(3-pyridiniobenzoimidazolium cations into a three-dimensional network via N—H...O hydrogen bonds. In addition, neighbouring diprotonated cations are arranged in a head-to-tail fashion with a plane-to-plane separation of 3.63 (10 Å, indicating the existence of weak aromatic π–π stacking interactions.

  4. 3-Ethyl-3-hy-droxy-8-meth-oxy-quinoline-2,4(1H,3H)-dione monohydrate.

    Science.gov (United States)

    Kafka, Stanislav; Pevec, Andrej; Proisl, Karel; Kimmel, Roman; Košmrlj, Janez

    2012-11-01

    In the title hydrate, C(12)H(13)NO(4)·H(2)O, the piperidine ring that is fused to the benzene ring is in a sofa conformation with the chiral C atom lying 0.4084 (18) Å out of the plane of the nine fused-ring atoms. In the crystal, O-H⋯O and N-H⋯O hydrogen bonds link the organic mol-ecules and water mol-ecules into chains running along the b-axis direction. The chains are further connected into layers parallel to the bc plane by π-π inter-actions between inversion-related benzene rings [centroid-centroid distance = 3.8846 (9) Å].

  5. 3-Hexadecyl-1,5-dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H-dione

    Directory of Open Access Journals (Sweden)

    Rachida Dardouri

    2011-05-01

    Full Text Available In the title molecule, C27H44N2O2, the seven-membered ring adopts a boat-shaped conformation, with two C atoms of the fused benzene ring forming the stern and the methine C atom forming the prow. The hexadecyl substituent occupies an equatorial position, with the aliphatic chain exhibibiting an extended zigzag conformation.

  6. (E-3-[(Dimethylaminomethylidene]-4-phenyl-1-(prop-2-ynyl-1H-1,5-benzodiazepin-2(3H-one

    Directory of Open Access Journals (Sweden)

    Mohamed Loughzail

    2014-01-01

    Full Text Available The title compound, C21H19N3O, exhibits an E configuration with respect to the C=C bond between the benzodiazepine and trimethylamine groups. The seven-membered diazepine ring displays a boat conformation. In the crystal, molecules are linked by a C—H...O hydrogen bond, forming a chain along [110].

  7. [Behavioral and electroencephalographic study of 7-chloro-1-methyl-5-phenyl-1 H-1,5-benzodiazepine-2,4-(3H,5H)-dione (clobazam)].

    Science.gov (United States)

    Gomita, Y; Morii, M; Ichimaru, Y; Moriyama, M; Ueki, S

    1983-10-01

    Behavioral and electroencephalographic effects of clobazam (CBZ), a 1, 5 benzodiazepine, were investigated in mice, rats and rabbits and compared with the effects of diazepam (DZP) and chlordiazepoxide (CDP). In EEG studies of rabbits, CBZ, DZP and CDP at doses of 2-10 mg/kg, i.v., caused a drowsy pattern, i.e., high voltage slow waves in the frontal cortex and the desynchronization of hippocampal theta wave. EEG arousal responses induced not only by auditory stimulation but also by electric stimulation of the mesencephalic reticular formation were inhibited by CBZ; CBZ was less potent than DZP, but more potent than CDP. On hypothalamic self-stimulation behavior of rats, low rate responses induced by low current brain stimulation, VI or DRL procedure were increased by oral administration of the three drugs. CBZ was less potent than DZP in the above respondings, but the same potency as CDP in VI or DRL responding and more potent in low rate responding induced by low current stimulation. The preventive effect of CBZ on MES convulsion in mice was less potent than DZP, but 2.5 times as potent as CDP. The preventive effect of CBZ was 1.3 times as potent as DZP and 2.5 times as potent as CDP. CBZ reduced the hyperemotionality of olfactory bulbectomized rats, and this effect was less than DZP in suppressing muricide. The muscle relaxant effect of CBZ in inclined screen and rotarod tests of mice was less than that of DZP. CBZ was 2.2 times as potent as CDP in potentiating thiopental sleep in mice, but less than DZP. These results indicate that CBZ is qualitatively similar to 1, 4 benzodiazepines, DZP and CDP, and is more potent than CDP, but less potent than DZP.

  8. 6-Bromo-1,3-di-2-propynyl-1H-imidazo[4,5-b]pyridin-2(3H-one

    Directory of Open Access Journals (Sweden)

    S. Dahmani

    2010-04-01

    Full Text Available The room-temperature reaction of propargyl bromide and 6-bromo-1,3-dihydroimidazo[4,5-b]pyridin-2-one in dimethylformamide yields the title compound, C12H8BrN3O, which features nitrogen-bound propynyl substituents. The imidazopyridine fused ring is almost planar (r.m.s. deviation = 0.011 Å; the propynyl chains point in opposite directions relative to the fused ring. One acetylenic H atom is hydrogen bonded to the carbonyl O atom of an inversion-related molecule, forming a dimer; adjacent dimers are linked by a second acetylene–pyridine C—H...N interaction, forming a layer motif.

  9. 3-({4-[(2-Methylbenzylideneamino]-5-sulfanylidene-1H-1,2,4-triazol-3-yl}methyl-1,3-benzoxazol-2(3H-one

    Directory of Open Access Journals (Sweden)

    Abdullah Aydın

    2013-02-01

    Full Text Available In the title compound, C18H15N5O2S, a weak intramolecular C—H...S hydrogen bond results in a small dihedral angle of 3.71 (9° between the methylphenyl and triazole rings, which, in turn, form dihedral angles of 80.09 (8 and 77.32 (8°, respectively, with the benzoxazolone mean plane. In the crystal, N—H...O hydrogen bonds link molecules into chains along [001], and weak C—H...N hydrogen bonds and π–π interactions between the five- and six-membered rings [centroid–centroid distances = 3.5074 (11 and 3.616 (1 Å] consolidate the crystal packing.

  10. KBS-3H layout adaptation 2007 for the Olkiluoto site

    Energy Technology Data Exchange (ETDEWEB)

    Johansson, Erik; Hagros, Annika; Autio, Jorma; Kirkkomaeki, Timo (Saanio and Riekkola Oy, Helsinki (Finland))

    2008-05-15

    As part of the KBS-3H design an Olkiluoto-specific layout of a KBS-3H repository has been produced based on the latest Olkiluoto data and the bedrock model. One of the main goals of this work was to support the evaluation of the feasibility of the one layer KBS-3H concept and to compare the layouts based on the KBS-3H and KBS-3V disposal concepts. The layout presented in this work can be considered only preliminary and involves a number of uncertainties. The percentage of unusable host rock was assumed to be 25% in this work but can change due to the further design of the different components of the KBS-3H disposal system and further development of the host rock criteria. The layout is also significantly affected by the layout-determining fracture zones. In this work 11 major (highly transmissive) fracture zones interpreted to intersect the -420 m level were considered deterministically. The KBS-3H layout requires a larger area than the KBS-3V repository and takes up most of the available area between the major fracture zones HZ20 and HZ21. This is mainly due to the long drift sections occupied by the compartment plugs (30 m) and the bentonite blocks in the blank zones (10 m), which reduces the usability of the host rock and results in larger canister spacings than in the KBS-3V concept, where the positioning of the deposition holes is very flexible and narrow zones with a moderate transmissivity usually have only a minor effect on the locations of the canisters. According to the results, there is enough bedrock in the current investigation area at central Olkiluoto for KBS-3H layout in one layer. However the layout takes up nearly all of the potential bedrock resource and therefore the result is quite sensitive to possible changes in the design bases

  11. Phylogenetic position and replication kinetics of Heliothis virescens ascovirus 3h (HvAV-3h isolated from Spodoptera exigua.

    Directory of Open Access Journals (Sweden)

    Guo-Hua Huang

    Full Text Available Insect-specific ascoviruses with a circular genome are distributed in the USA, France, Australia and Indonesia. Here, we report the first ascovirus isolation from Spodoptera exigua in Hunan, China. DNA-DNA hybridization to published ascoviruses demonstrated that the new China ascovirus isolate is a variant of Heliothis virescens ascovirus 3a (HvAV-3a, thus named HvAV-3h. We investigated the phylogenetic position, cell infection, vesicle production and viral DNA replication kinetics of HvAV-3h, as well as its host-ranges. The major capsid protein (MCP gene and the delta DNA polymerase (DNA po1 gene of HvAV-3h were sequenced and compared with the available ascovirus isolates for phylogenetic analysis. This shows a close relationship with HvAV-3g, originally isolated from Indonesia, HvAV-3e from Australia and HvAV-3c from United States. HvAV-3h infection induced vesicle production in the SeE1 cells derived from S. exigua and Sf9 cells derived from S. frugiperda, resulting in more vesicles generated in Sf9 than SeE1. Viral DNA replication kinetics of HvAV-3h also demonstrated a difference between the two cell lines tested. HvAV-3h could readily infect three important insect pests Helicoverpa armigera (Hübner, Spodoptera exigua (Hübner and Spodoptera litura (Fabricius from two genera in different subfamilies with high mortalities.

  12. Depolarization-induced release of [(3)H]D-aspartate from GABAergic neurons caused by reversal of glutamate transporters

    DEFF Research Database (Denmark)

    Jensen, J B; Pickering, D S; Schousboe, A

    2000-01-01

    by addition of cobalt. Since AMPA has a rapid desensitizing effect on AMPA receptors, it was examined whether AMPA under non-desensitizing conditions was able to induce an increased release of [(3)H]D-aspartate as compared to the conditions of applying AMPA alone. The desensitization of AMPA receptors...... was blocked by 6-chloro-3,4-dihydro-3-(2-norbornen-5-yl)-2H-1,2, 4-benzothiadiazine-7-sulphonamide-1,1-dioxide (cyclothiazide). Under the non-desensitizing conditions, the AMPA-induced release of [(3)H]D-aspartate was highly enhanced showing about a 10-fold increase over basal release. Addition of cobalt...... or lanthanum did not decrease the amount of [(3)H]D-aspartate released, indicating that the release originated from a cytoplasmic pool. Kainate, which induces an almost non-desensitizing effect on AMPA receptors, showed similar results as observed for AMPA under non-desensitizing conditions. The NMDA receptor...

  13. Synthesis and biological activity of novel series of 1,3-benzoxazol-2(3H)-one derivatives.

    Science.gov (United States)

    Krawiecka, Mariola; Kuran, Bozena; Kossakowski, Jerzy; Kierzkowska, Marta; Młynarczyk, Grazyna; Cieślak, Marcin; Kaźmierczak-Barańska, Julia; Królewska, Karolina; Dobrowolski, Michał A

    2013-01-01

    In the search for novel biological agents, a series of new derivatives N-substituted 1,3-benzoxazol-2(3H)-one, 5-chloro-1,3-benzoxazol-2(3H)-one, 6-bromo-1,3-benzoxazol-2(3H)-one were prepared. All of the compounds were characterized by 1H NMR, 13C NMR and ESI MS spectra. Moreover, for compound 1 an Xray structure was determined. All derivatives were tested for antimicrobial activity against a selection of Gram-positive, Gram-negative bacteria and yeasts. The selected compounds (2-8, 10) were tested for their cytotoxic properties in K562, HeLa and normal cells.

  14. Synthesis and Antiviral Bioactivities of 2-Aryl- or 2-Methyl-3-(substituted- Benzalamino-4(3H-quinazolinone Derivatives

    Directory of Open Access Journals (Sweden)

    Zhuo Chen

    2007-12-01

    Full Text Available A simple and general method has been developed for the synthesis of various4(3H-quinazolinone derivatives by the treatment of the appropriate 3-amino-2-aryl-4(3H-quinazolinone with a substituted benzaldehyde in ethanol. The structures of the compoundswere characterized by elemental analysis, IR, 1H-NMR and 13C-NMR spectra. The title 2-aryl- or 2-methyl-3-(substituted-benzalamino-4(3H-quinazolinone compounds III-1~III-31 were found to possess moderate to good antiviral activity. Semi-quantitative PCR andReal Time PCR assays were used to ascertain the target of action of compound III-31against TMV. The studies suggest that III-31 possesses antiviral activity due to inductionof up-regulation of PR-1a and PR-5, thereby inhibiting virus proliferation and movementby enhancement of the activity of some defensive enzyme.

  15. Novel Synthesis of Tryptamine Derived 4-Hydroxy-4-arylthiazolidine-2-thiones and 4-Arylthiazole-2(3H)-thiones by Multicomponent Reactions

    Energy Technology Data Exchange (ETDEWEB)

    Devi, Nepram Sushuma; Singh, Sarangthem Joychandra; Singh, Okram Mukherjee [Manipur Univ., Imphal (India); Mahiya, Kuldeep [Chaudhary Devi Lal Univ., Sirsa (India); Choi, Hojune; Lee, Sang Gyeong [Research Institute of Natural Science, Gyeongsang National Univ., Jinju (Korea, Republic of)

    2016-09-15

    An efficient one-pot multicomponent synthesis of 3-(2-(1H-indol-3-yl)ethyl)-4-hydroxy-4-arylthiazolidine-2-thione and 3-(2-(1H-indol-3-yl)ethyl)-4-arylthiazole-2(3H)-thione has been developed from a multicomponent reaction of tryptamine, carbon disulfide and phenacyl bromide. This protocol has an advantage such as operational simplicity, short reaction time, and affording good to excellent yields.

  16. Design and Synthesis of Novel 5-Sulfoxide-substituted Pyrazolo[5,1-d] [1,2,3,5]tetrazin-4(3H)ones

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    A series of novel 5-sulfoxide-substituted pyrazolo[5,1-d][1,2,3,5]tetrazin-4(3H)ones 4a-j were designed and efficiently synthesized via a diazotization of 5-amine-3-methylsulfinyl1H-pyrazole, followed by cycloaddition with aryl isocyanate. A possible reaction mechanism is outlined and discussed. These new compounds exhibit some biological activity as preliminary bioassay indicated. Their structures were confirmed with1 H NMR, IR and elemental analysis.

  17. Analysis list: Nr1h3 [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available Nr1h3 Liver + mm9 http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h3.1.tsv... http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h3.5.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h...3.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Nr1h3.Liver.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Liver.gml ...

  18. Analysis list: Nr1h2 [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available Nr1h2 Blood + mm9 http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h2.1.tsv... http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h2.5.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Nr1h...2.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Nr1h2.Blood.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Blood.gml ...

  19. An elevated 1-h post- load glucose level during the oral glucose tolerance test detects prediabetes.

    Science.gov (United States)

    Buysschaert, Martin; Bergman, Michael; Yanogo, Donald; Jagannathan, Ram; Buysschaert, Benoit; Preumont, Vanessa

    The objective of the study was to compare the diagnosis of dysglycemic states by conventional oral glucose tolerance test (OGTT) criteria (fasting and 2-h plasma glucose) with the 1-h post-load plasma glucose level. 34 individuals (mean age: 55±13years; BMI: 27.7±6.3kg/m(2)) at risk for prediabetes were administered a 75g OGTT. Individuals with normal glucose tolerance (NGT) or prediabetes were identified according to fasting and/or 2-h plasma glucose (PG) concentrations. Subsequently, subjects were divided in 2 groups: group 1 (n=21) with a 1-h PGh PG≥155mg/dl. HOMA was performed to assess β-cell function and insulin sensitivity. NGT or prediabetes based on conventional criteria correlated with the 1-h PGh PG≥155mg/dl was associated with higher HbA1c levels (6.1±0.5 vs. 5.5±0.3%, ph PGh post-load plasma glucose value ≥155mg/dl is strongly associated with conventional criteria for (pre)diabetes and alterations of β-cell function. Copyright © 2016 Diabetes India. Published by Elsevier Ltd. All rights reserved.

  20. Studies on (/sup 3/H) hemicholinium-3 ((/sup 3/H)HC-3), (/sup 3/H) pirenzepine ((/sup 3/H)PZ) and (/sup 3/H)(-)quinuclidinyl benzilate ((/sup 3/H)(-)QNB) binding with choline and acetylcholine analogues (AF30, AF64, AF64A)

    Energy Technology Data Exchange (ETDEWEB)

    Gulva, K.; Fisher, A.; Hanin, I.; Yamamura, H.I.

    1986-03-05

    Choline deficiency in brain function has been implicated in several neurological disorders. Therefore, the usefulness of choline and its analogues as therapeutic agents or potential tools in developing selective models of central cholinergic hypofunction has been under investigation. The inhibitory potencies of ethylcholine mustard (AF64) and ethylcholine mustard aziridium (AF64A) were tested in inhibiting specific (/sup 3/H)HC-3 (rat striatal membranes), (/sup 3/H)PZ and (/sup 3/H)(-)QNB (cortical and heart membranes). AF64 and AF64A inhibited the binding of (/sup 3/H)HC-3 with low affinity. Results for one-site fit are: AF64: IC/sub 50/ = 107 ..mu..M, n/sub H/ = 0.62; AF64A: IC/sub 50/ = 130 ..mu..M, n/sub H/ = 0.56. Two site-fit resulted IC/sub 50/ values of 11-12 ..mu..M for high affinity and 360-730 ..mu..M for low affinity (relative proportions: 45% and 55%, respectively) in both cases. AF30 (a rigid choline analogue with agonist activity), AF64 and AF64A were weak inhibitors of muscarinic receptor bindings with IC/sub 50/ values in the micromolar range in both cortical and heart membranes, although AF64A showed ten-fold higher affinity in inhibiting (/sup 3/H)PZ binding than (/sup 3/H)(-)QNB binding in cortical membranes.

  1. Volumetric Properties of the Mixture Iodoethane C2H5I + C3H7Br 1-Bromopropane (LB0775, VMSD1212)

    Science.gov (United States)

    Cibulka, I.; Hnědkovský, L.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume A `Binary Liquid Systems of Nonelectrolytes' of Volume 23 `Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV `Physical Chemistry'. It corresponds to the data set LB0775 of the ELBT database.

  2. Volumetric Properties of the Mixture Iodoethane C2H5I + C3H7Br 1-Bromopropane (LB0772, VMSD1111)

    Science.gov (United States)

    Cibulka, I.; Hnědkovský, L.; Fontaine, J.-C.; Sosnkowska-Kehiaian, K.; Kehiaian, H. V.

    This document is part of Subvolume A `Binary Liquid Systems of Nonelectrolytes' of Volume 23 `Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV `Physical Chemistry'. It corresponds to the data set LB0772 of the ELBT database.

  3. Evaporation and concentration gradients created by episodic river recharge in a semi-arid zone aquifer: Insights from Cl-, δ18O, δ2H, and 3H

    Science.gov (United States)

    Meredith, K. T.; Hollins, S. E.; Hughes, C. E.; Cendón, D. I.; Chisari, R.; Griffiths, A.; Crawford, J.

    2015-10-01

    This study has significantly advanced our understanding of the origin of groundwater recharge in a semi-arid zone region of the Darling River catchment, Australia. The generally accepted hypothesis in arid zone environments in Australia that river water forms the primary groundwater recharge source has proven difficult to monitor. This is due to the time lags between large floods, the remoteness and expense of studying these hydrologically complex systems in detail. In addition, the highly episodic nature of dryland rivers complicates the interpretation of the groundwater signal. A range of hydrochemical tracers (chloride, oxygen-18, deuterium and tritium) measured in rain, river water, soil water and groundwater were used in this multi-year study to trace the pathways of groundwater recharge under wet and dry climatic conditions. The evaporation and Cl concentrations observed in the unsaturated zone confirmed that small volumetric inputs from periodic rainfall were not the major recharge mechanism. Sampling which included an overbank flooding event in March 2012 provided firm evidence for groundwater originating from high flow episodic river recharge. The use of long-term environmental data to understand how economically important water resources respond to climate change with increasing temperatures is considered essential for future sustainability.

  4. EPR and optical investigation of VO(II) in Zn(C3H3O4)2(H2O)2 single crystals: An interstitial site

    Science.gov (United States)

    Natarajan, B.; Mithira, S.; Deepa, S.; Sambasivarao, P.

    2007-10-01

    EPR spectroscopic investigations on single crystals of diaquabis[malonato(1-)-κ2O,O‧] zinc(II) doped with VO(II) ion have been carried out at X-band frequencies and at 300 K. The single crystal, rotated along the three mutually orthogonally axes, has yielded spin-Hamiltonian parameters g and A as: gxx=1.980, gyy=1.972, gzz=1.937 and Axx=8.4, Ayy=6.1, Azz=18.1 mT, respectively. These spin-Hamiltonian parameters reflect a slight deviation from axial symmetry to rhombic, which is elucidated by the interstitial occupation of vanadyl ions. The isofrequency plots and powder EPR spectrum have been simulated. The percentage of metal-oxygen bond has been estimated. The optical absorption spectrum exhibits four bands at 257, 592, 720 and 764 nm suggesting a C4v symmetry. The admixture coefficients and bonding parameters have also been calculated by collaborating EPR data with optical data.

  5. Ab initio studies of O2-(H2O)n and O3-(H2O)n anionic molecular clusters, n≤12

    DEFF Research Database (Denmark)

    Bork, Nicolai Christian; Kurtén, T.; Enghoff, Martin Andreas Bødker

    2011-01-01

    An ab initio study of gaseous clusters of O2− and O2− with water is presented. Based on thorough scans of configurational space, we determine the thermodynamics of cluster growth. The results are in good agreement with benchmark computational methods and existing experimental data. We find...

  6. Water-Isotopes (2H, 3H, 18O) to trace the source and timing of recharge in a fractured granite aquifer in Western Kenya, Africa

    Science.gov (United States)

    Kralik, Martin; Whylidal, Stefan; Asunah, Francis; Sültenfuß, Jürgen

    2014-05-01

    The Vihiga District in West Kenya North-West of Lake Victoria is one of the most densely populated areas in Kenya with 1033 person per square kilometer. To find the most suitable location of an own well for a Primary School in this district, springs, school wells and creeks were sampled in the surroundings to get information about the hydrological cycle in the area. The Waluka Primary school (0.02134°N, 34.64311°E) is situated on the northern slope of the Maragoli Hills 20 km to the North-West of the Nyanzan provincial capital of Kisumu at the eastern shore of Lake Victoria. The hilly relief varies between 1535 - 1675m. The yearly precipitation is between 1200-1600 mm/a (23°C mean temperature) with biannual rainy seasons in which the long rains are generally from March to May as the Inter-Tropical Convergence Zone (ITCZ) moves northwards, and the short rains are typically from October to December as the ITCZ retreats southwards. A lateritic soil covers a thin alteration zone above the Precambrian Maragoli-Granite (Saggerson, 1952). Water circulates either in the thin alteration zone or in fault zones cutting through the Precambrian granite. From discharge measurements of two springs and a creek at the end of the dry season (February 2012) a minimum discharge of ca. 10-20 L/s km2 (300-600 mm) can be estimated. The water is of the alkaline sulfate-nitrate type with low mineralization (70-150 μ S/cm, 25°C) and a low pH of about 5 to 6. The delta oxygen-18 and deuterium value ranges between -2.84 to -1.98 oand -8.5 to - 3.9 o(VSMOW). The deuterium excess ranges from 11.7-14.2 oThe water of one spring and well close to the school have a tritium content of 1.42 - 1.62 TU. All groundwater has a low arsenium, fluorine and uranium content, which had only a short soil passage. The relatively elevated, but not problematic content in nitrate (10 - 16 mg/L) probaly reflects the intensive agricultural activities in this area. As the mean δ 18O values during the rainy seasons are significantly lower (-3 to -4 o) than in the mean precipitation during the rest of the year (-2.5 to -1.9 o; Mwango, 2003) one can conclude that the main spring 'Anzaya' and the well in the Naboka Secondary School are recharged from deeper faults with water supplied more during the rainy season. The slightly higher d-excess of 13.4-14.2 ocompared to 11.7-12.6 oin the rest of the samples, indicates a somewhat higher recharge area of this two sites with water vapor recycled in the precipitation around the Liailhunuu peak (ca. 1675m). This effect is also supported by spring-water measurements at the Kilimanjaro (d-excess 13.4-6.6 o) 400 km SE. Similarily, the tritium content of 1.42 - 1.62 TU indicate that compared to a mean tritium content of 2 TU in the rain of this area (Mwango, 2003) the mean residence time can be in the range of recent to few years only.

  7. Synthesis of singly /sup 2/H-, /sup 3/H-, and /sup 14/C- and doubly labeled acetaminophen, phenacetin, and p-acetanisidine

    Energy Technology Data Exchange (ETDEWEB)

    Chan, K.K. (University of Southern California, Los Angeles (USA)); Pang, K.S. (Houston Univ., TX (USA))

    1982-03-01

    Several efficient procedures for the synthesis of deuterium, tritium, and /sup 14/C-labeled acetaminophen, phenacetin, and p-acetanisidine are described. p-Aminophenol was acylated by the appropriate acetic anhydride under mild conditions yielding labeled acetaminophen. With O-alkylation using NaCH/sub 2/SOCH/sub 3/ and appropriate labeled and unlabeled alkyl halides, labeled phenacetin and p-acetanisidine were also obtained. Phenacetin labeled both with /sup 14/C on the acyl group and deuterium on the ethoxy group was synthesized in high yield by acylation of p-phenetidine-d/sub 5/. The last compound was obtained by acid hydrolysis of phenacetin-d/sub 5/ synthesized previously.

  8. Calculational and Experimental Investigations of the Pressure Effects on Radical - Radical Cross Combinations Reactions: C2H5 + C2H3

    Science.gov (United States)

    Fahr, Askar; Halpern, Joshua B.; Tardy, Dwight C.

    2007-01-01

    Pressure-dependent product yields have been experimentally determined for the cross-radical reaction C2H5 + C2H3. These results have been extended by calculations. It is shown that the chemically activated combination adduct, 1-C4H8*, is either stabilized by bimolecular collisions or subject to a variety of unimolecular reactions including cyclizations and decompositions. Therefore the "apparent" combination/disproportionation ratio exhibits a complex pressure dependence. The experimental studies were performed at 298 K and at selected pressures between about 4 Torr (0.5 kPa) and 760 Torr (101 kPa). Ethyl and vinyl radicals were simultaneously produced by 193 nm excimer laser photolysis of C2H5COC2H3 or photolysis of C2H3Br and C2H5COC2H5. Gas chromatograph/mass spectrometry/flame ionization detection (GC/MS/FID) were used to identify and quantify the final reaction products. The major combination reactions at pressures between 500 (66.5 kPa) and 760 Torr are (1c) C2H5 + C2H3 yields 1-butene, (2c) C2H5 + C2H5 yields n-butane, and (3c) C2H3 + C2H3 yields 1,3-butadiene. The major products of the disproportionation reactions are ethane, ethylene, and acetylene. At moderate and lower pressures, secondary products, including propene, propane, isobutene, 2-butene (cis and trans), 1-pentene, 1,4-pentadiene, and 1,5-hexadiene are also observed. Two isomers of C4H6, cyclobutene and/or 1,2-butadiene, were also among the likely products. The pressure-dependent yield of the cross-combination product, 1-butene, was compared to the yield of n-butane, the combination product of reaction (2c), which was found to be independent of pressure over the range of this study. The [ 1-C4H8]/[C4H10] ratio was reduced from approx.1.2 at 760 Torr (101 kPa) to approx.0.5 at 100 Torr (13.3 kPa) and approx.0.1 at pressures lower than about 5 Torr (approx.0.7 kPa). Electronic structure and RRKM calculations were used to simulate both unimolecular and bimolecular processes. The relative importance

  9. Synthesis and characterization of d10 metal complexes with mixed 1,3-di(1H-imidazol-4-yl)benzene and multicarboxylate ligands

    Science.gov (United States)

    Chen, Zhi-Hao; Zhao, Yue; Chen, Shui-Sheng; Wang, Peng; Sun, Wei-Yin

    2013-06-01

    Seven new coordination polymers [Zn(H2L)(mbdc)] (1), [Zn(H3L)(btc)] (2), [Zn(H2L)(Hbtc)] (3), [Zn(H2L)(Hbtc)]·H2O (4), [Zn2(H2L)(btc)(μ2-OH)] (5), [Cd(H2L)(mbdc)] (6) and [Cd3(H2L)2(btc)2(H2O)]·5H2O (7) were synthesized by reactions of the corresponding metal salt with rigid ligand 1,3-di(1H-imidazol-4-yl)benzene (H2L) and different carboxylic acids of 1,3-benzenedicarboxylic acid (H2mbdc) and benzene-1,3,5-tricarboxylic acid (H3btc), respectively. The results of X-ray crystallographic analysis indicate that complex 1 is 1D chain while 2 is a (3,3)-connected 2D network with Point (Schläfli) symbol of (4,82). Complexes 3 and 6 are 2D networks, 4 is a 3-fold interpenetrating 3D framework with Point (Schläfli) symbol of (65,8) and 5 is a (3,8)-connected 2D network with Point (Schläfli) symbol of (3,42)2(34,46,56,68,73,8), while 7 is a (3,10)-connected 3D net with Schläfli symbol of (3,4,5)2(34,48,518,612,72,8). The thermal stability and photoluminescence of the complexes were investigated. Furthermore, DFT calculations were performed for 2-4 to discuss the temperature controlled self-assembly of the complexes.

  10. Cd(II) and Co(II) coordination polymers constructed from benzene-1,4-dicarboxylic acid and 2-(pyridin-3-yl)-1H-benzimidazole ligands.

    Science.gov (United States)

    Chen, Xiao-Hua; Huang, Hua; Yang, Ming-Xing; Chen, Li-Juan; Lin, Shen

    2014-05-01

    In poly[aqua(μ3-benzene-1,4-dicarboxylato-κ(5)O(1),O(1'):O(1):O(4),O(4'))[2-(pyridin-3-yl-κN)-1H-benzimidazole]cadmium(II)], [Cd(C8H4O4)(C12H9N3)(H2O)]n, (I), each Cd(II) ion is seven-coordinated by the pyridine N atom from a 2-(pyridin-3-yl)benzimidazole (3-PyBIm) ligand, five O atoms from three benzene-1,4-dicarboxylate (1,4-bdc) ligands and one O atom from a coordinated water molecule. The complex forms an extended two-dimensional carboxylate layer structure, which is further extended into a three-dimensional network by hydrogen-bonding interactions. In catena-poly[[diaquabis[2-(pyridin-3-yl-κN)-1H-benzimidazole]cobalt(II)]-μ2-benzene-1,4-dicarboxylato-κ(2)O(1):O(4)], [Co(C8H4O4)(C12H9N3)2(H2O)2]n, (II), each Co(II) ion is six-coordinated by two pyridine N atoms from two 3-PyBIm ligands, two O atoms from two 1,4-bdc ligands and two O atoms from two coordinated water molecules. The complex forms a one-dimensional chain-like coordination polymer and is further assembled by hydrogen-bonding interactions to form a three-dimensional network.

  11. Phenyl Ring-Substituted Lobelane Analogs: Inhibition of [3H]Dopamine Uptake at the Vesicular Monoamine Transporter-2

    Science.gov (United States)

    Nickell, Justin R.; Zheng, Guangrong; Deaciuc, Agripina G.; Crooks, Peter A.

    2011-01-01

    Lobeline attenuates the behavioral effects of methamphetamine via inhibition of the vesicular monoamine transporter (VMAT2). To increase selectivity for VMAT2, chemically defunctionalized lobeline analogs, including lobelane, were designed to eliminate nicotinic acetylcholine receptor affinity. The current study evaluated the ability of lobelane analogs to inhibit [3H]dihydrotetrabenazine (DTBZ) binding to VMAT2 and [3H]dopamine (DA) uptake into isolated synaptic vesicles and determined the mechanism of inhibition. Introduction of aromatic substituents in lobelane maintained analog affinity for the [3H]DTBZ binding site on VMAT2 and inhibitory potency in the [3H]DA uptake assay assessing VMAT2 function. The most potent (Ki = 13–16 nM) analogs in the series included para-methoxyphenyl nor-lobelane (GZ-252B), para-methoxyphenyl lobelane (GZ-252C), and 2,4-dichlorphenyl lobelane (GZ-260C). Affinity of the analogs for the [3H]DTBZ binding site did not correlate with inhibitory potency in the [3H]DA uptake assay. It is noteworthy that the N-benzylindole-, biphenyl-, and indole-bearing meso-analogs 2,6-bis[2-(1-benzyl-1H-indole-3-yl)ethyl]-1-methylpiperidine hemifumarate (AV-1-292C), 2,6-bis(2-(biphenyl-4-yl)ethyl)piperidine hydrochloride (GZ-272B), and 2,6-bis[2-(1H-indole-3-yl)ethyl]-1-methylpiperidine monofumarate (AV-1-294), respectively] inhibited VMAT2 function (Ki = 73, 127, and 2130 nM, respectively), yet had little to no affinity for the [3H]DTBZ binding site. These results suggest that the analogs interact at an alternate site to DTBZ on VMAT2. Kinetic analyses of [3H]DA uptake revealed a competitive mechanism for 2,6-bis(2-(4-methoxyphenyl)ethyl)piperidine hydrochloride (GZ-252B), 2,6-bis(2-(4-methoxyphenyl)ethyl)-1-methylpiperidine hydrochloride (GZ-252C), 2,6-bis(2-(2,4-dichlorophenyl)ethyl)piperidine hydrochloride (GZ-260C), and GZ-272B. Similar to methamphetamine, these analogs released [3H]DA from the vesicles, but with higher potency. In contrast to

  12. Aberrant 3H in Ehrlich mouse ascites tumor cell nucleotides after in vivo labeling with myo-[2-3H]- and L -myo-[1-3H]inositol: implications for measuring inositol phosphate signaling

    DEFF Research Database (Denmark)

    Christensen, Søren C.; Jensen, Annelie Kolbjørn; Simonsen, L.O.

    2003-01-01

    : the oxidative conversion to -glucuronate. In contrast, with the 3H at C2 of myo-inositol, the 3H-C2 passes into the pentose phosphate conversions with resulting labeling of nucleotides. The extent of catabolism to 3H-labeled water, the cellular accumulation of 3H-myo-inositol, the incorporation into cellular...

  13. Synthesis of [4,6-{sup 3}H]-2-pyridone and [{sup 3}H]-RS-91309

    Energy Technology Data Exchange (ETDEWEB)

    Keczer, S. de; Parnes, Howard [Syntex Discovery Research, Palo Alto, CA (United States)

    1995-12-31

    We describe herein, a novel synthesis of the previously unreported compound, 4,6-dibromo-2-pyridone (3) and its use in the preparation of [{sup 3}H]-RS-91309, a potassium channel modulator. This key intermediate, (3), was reduced with carrier free tritium gas to furnish [4,6-{sup 3}H]-2-pyridone (9) having a specific activity of 50 Ci/mmole. Condensation of (9) with epoxide (10), followed by elaboration of the resulting chromene methyl group of (12) gave [{sup 3}H]-RS-91309 (14) whose specific activity was also 50 Ci/mmole. This chemistry, as well as the solution of several micro-scale related stoichiometry problems is discussed. (Author).

  14. SPATIALLY RESOLVED l-C{sub 3}H{sup +} EMISSION IN THE HORSEHEAD PHOTODISSOCIATION REGION: FURTHER EVIDENCE FOR A TOP-DOWN HYDROCARBON CHEMISTRY

    Energy Technology Data Exchange (ETDEWEB)

    Guzmán, V. V.; Öberg, K. I. [Harvard-Smithsonian Center for Astrophysics, 60 Garden Street, Cambridge, MA 02138 (United States); Pety, J. [Institut de Radioastronomie Millimétrique (IRAM), 300 rue de la Piscine, F-38406 Saint Martin d’Hères (France); Goicoechea, J. R. [Instituto de Ciencia de Materiales de Madrid (CSIC), E-28049 Cantoblanco, Madrid (Spain); Gerin, M. [LERMA, Observatoire de Paris, École Normale Supérieure, PSL Research University, CNRS, UMR8112, F-75014 Paris (France); Roueff, E. [Sorbonne Universités, UPMC Univ. Paris 06, UMR8112, LERMA, F-75005 Paris (France); Gratier, P., E-mail: vguzman@cfa.harvard.edu [Université de Bordeaux, LAB, UMR 5804, F-33270, Floirac (France)

    2015-02-20

    Small hydrocarbons, such as C{sub 2}H, C{sub 3}H, and C{sub 3}H{sub 2} are more abundant in photo-dissociation regions (PDRs) than expected based on gas-phase chemical models. To explore the hydrocarbon chemistry further, we observed a key intermediate species, the hydrocarbon ion l-C{sub 3}H{sup +}, in the Horsehead PDR with the Plateau de Bure Interferometer at high-angular resolution (6″). We compare with previous observations of C{sub 2}H and c-C{sub 3}H{sub 2} at similar angular resolution and new gas-phase chemical model predictions to constrain the dominant formation mechanisms of small hydrocarbons in low-UV flux PDRs. We find that at the peak of the HCO emission (PDR position), the measured l-C{sub 3}H{sup +}, C{sub 2}H, and c-C{sub 3}H{sub 2} abundances are consistent with current gas-phase model predictions. However, in the first PDR layers, at the 7.7 μm polycyclic aromatic hydrocarbon band emission peak, which are more exposed to the radiation field and where the density is lower, the C{sub 2}H and c-C{sub 3}H{sub 2} abundances are underestimated by an order of magnitude. At this position, the l-C{sub 3}H{sup +} abundance is also underpredicted by the model but only by a factor of a few. In addition, contrary to the model predictions, l-C{sub 3}H{sup +} peaks further out in the PDR than the other hydrocarbons, C{sub 2}H and c-C{sub 3}H{sub 2}. This cannot be explained by an excitation effect. Current gas-phase photochemical models thus cannot explain the observed abundances of hydrocarbons, in particular, in the first PDR layers. Our observations are consistent with a top-down hydrocarbon chemistry, in which large polyatomic molecules or small carbonaceous grains are photo-destroyed into smaller hydrocarbon molecules/precursors.

  15. Modelling two-phase transport of 3H/3He

    NARCIS (Netherlands)

    Visser, A.; Schaap, J.D.; Leijnse, T.; Broers, H.P.; Bierkens, M.F.P.

    2008-01-01

    Degassing of groundwater by excess denitrification of agricultural pollution complicates the interpretation of 3H/3He data and hinders the estimation of travel times in nitrate pollution studies. In this study we used a two-phase flow and transport model (STOMP) to evaluate the method presented by

  16. Modelling two-phase transport of 3H/3He

    NARCIS (Netherlands)

    Visser, A.; Schaap, J.D.; Leijnse, T.; Broers, H.P.; Bierkens, M.F.P.

    2008-01-01

    Degassing of groundwater by excess denitrification of agricultural pollution complicates the interpretation of 3H/3He data and hinders the estimation of travel times in nitrate pollution studies. In this study we used a two-phase flow and transport model (STOMP) to evaluate the method presented by V

  17. Synthesis of [12-{sup 3}H]-(+-)-Calanolide A

    Energy Technology Data Exchange (ETDEWEB)

    Rehder, K.S.; Hristova-Kazmierski, M.K.; Kepler, J.A. [Research Triangle Inst., Research Triangle Park, NC (United States). Organic and Medicinal Chemistry

    1996-12-01

    [12-{sup 3}H]-({+-})-Calanolide A (9) was synthesized in five steps from readily available phloroglucinol. Stereoselective Luche reduction of trans-ketone with cerium(III) chloride and sodium borotritide in methanol gave 338 {mu}Ci of 9 with a specific activity of 63.0 mCi/mmol. (author).

  18. Dating degassed groundwater with 3H/3He

    NARCIS (Netherlands)

    Visser, A.; Broers, H.P.; Bierkens, M.F.P.

    2007-01-01

    The production of gases in groundwater under contaminated locations by geochemical and biological processes is not uncommon. Degassing of these gases from groundwater and repartitioning of noble gases between water and gas phase distorts groundwater dating by 3H/3He. We observed noble gas concentrat

  19. Dating degassed groundwater with 3H/3He

    NARCIS (Netherlands)

    Visser, A.; Broers, H.P.; Bierkens, M.F.P.

    2007-01-01

    The production of gases in groundwater under contaminated locations by geochemical and biological processes is not uncommon. Degassing of these gases from groundwater and repartitioning of noble gases between water and gas phase distorts groundwater dating by 3H/3He. We observed noble gas

  20. Structure-function studies of histone H3/H4 tetramer maintenance during transcription by chaperone Spt2.

    Science.gov (United States)

    Chen, Shoudeng; Rufiange, Anne; Huang, Hongda; Rajashankar, Kanagalaghatta R; Nourani, Amine; Patel, Dinshaw J

    2015-06-15

    Cells use specific mechanisms such as histone chaperones to abrogate the inherent barrier that the nucleosome poses to transcribing polymerases. The current model postulates that nucleosomes can be transiently disrupted to accommodate passage of RNA polymerases and that histones H3 and H4 possess their own chaperones dedicated to the recovery of nucleosomes. Here, we determined the crystal structure of the conserved C terminus of human Suppressors of Ty insertions 2 (hSpt2C) chaperone bound to an H3/H4 tetramer. The structural studies demonstrate that hSpt2C is bound to the periphery of the H3/H4 tetramer, mimicking the trajectory of nucleosomal-bound DNA. These structural studies have been complemented with in vitro binding and in vivo functional studies on mutants that disrupt key intermolecular contacts involving two acidic patches and hydrophobic residues on Spt2C. We show that contacts between both human and yeast Spt2C with the H3/H4 tetramer are required for the suppression of H3/H4 exchange as measured by H3K56ac and new H3 deposition. These interactions are also crucial for the inhibition of spurious transcription from within coding regions. Together, our data indicate that Spt2 interacts with the periphery of the H3/H4 tetramer and promotes its recycling in the wake of RNA polymerase. © 2015 Chen et al.; Published by Cold Spring Harbor Laboratory Press.

  1. Analysis list: NR1H3 [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available NR1H3 Adipocyte,Blood + hg19 http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/target.../NR1H3.1.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/target/NR1H3.5.tsv http://dbarchive.bioscienced...bc.jp/kyushu-u/hg19/target/NR1H3.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/colo/NR1H3.Adipocyte....tsv,http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/colo/NR1H3.Blood.tsv http://dbarchive.bioscience...dbc.jp/kyushu-u/hg19/colo/Adipocyte.gml,http://dbarchive.biosciencedbc.jp/kyushu-u/hg19/colo/Blood.gml ...

  2. Crystal structure of 2-methyl-1H-imidazol-3-ium hydrogen oxalate dihydrate

    Directory of Open Access Journals (Sweden)

    Mouhamadou Birame Diop

    2016-08-01

    Full Text Available Single crystals of the title molecular salt, C4H7N2+·HC2O4−·2H2O, were isolated from the reaction of 2-methyl-1H-imidazole and oxalic acid in a 1:1 molar ratio in water. In the crystal, the cations and anions are positioned alternately along an infinite [010] ribbon and linked together through bifurcated N—H...(O,O hydrogen bonds. The water molecules of crystallization link the chains into (10-1 bilayers, with the methyl groups of the cations organized in an isotactic manner.

  3. 4-Amino-1H-1,2,4-triazol-1-ium nitrate

    Directory of Open Access Journals (Sweden)

    Ivan Němec

    2011-01-01

    Full Text Available The non-centrosymmetric crystal structure of the novel semi-organic title compound, C2H5N4+·NO3−, is based on alternating layers of 4-amino-1H-1,2,4-triazolinium cations (formed by parallel chains of cations mediated by weak C—H...N hydrogen bonds and nitrate anions interconnected via linear and bifurcated N—H...O hydrogen bonds and weak C—H...O hydrogen bonds. N—H...N hydrogen bonds link the anions and cations.

  4. Research on the degradation 1,2,4-trichlorobenzene by O3/H2O2/UV process%O3/H2O2/UV降解1,2,4-三氯苯的研究

    Institute of Scientific and Technical Information of China (English)

    孙云娜; 魏东洋; 陆桂英; 贾晓珊; 李杰; 许振成

    2013-01-01

    采用O3/H2O2/UV工艺处理1,2,4-三氯苯(TCB)模拟废水,考察了TCB初始浓度、pH、H2O2投加量及O3转化率等因素对O3/H2O2/UV降解TCB的影响,推断了TCB可能的降解途径.结果表明:(1)H2O2、O3、UV、O3/H2O2、O3/H2 O2/UV 5种体系对TCB的降解效果为H2O2 <UV<O3 <O3/H2O2 <O3/H2O2/UV.(2)O3/H2O2/UV对TCB降解的单因素实验表明,TCB初始浓度越小、O3转化率越高,TCB去除率越大;H2O2的投加量存在一个最佳值,低于或高于这个最佳值都会导致TCB去除率的下降;在碱性条件下,TCB的降解效果更佳.(3)推测O3/H2O2/UV工艺降解TCB的机制主要为TCB与·OH的反应过程,其历程可分为3步:反应初期阶段,苯环上的C-Cl被·OH攻击,产生羟基化氯苯化合物;苯环得到活化,·OH进攻苯环,产生低氯代苯类物质;羟基化合物破环,生成小分子有机酸.%The O3/H2O2/UV combination process was employed to treat the simulated 1,2,4-trichlorobenzene (TCB) containing wastewater. The effect of initial TCB concentration, pH, H2O2 dosage and ozone transform rate on TCB removal efficiency was investigated. The potential degradation pathway of TCB was proposed with the help of GC,GC/MS and HPLC analysis. Results showed that the removal efficiency of TCB in 5 degradation system (H2O2 , O3,UV,O3/H2O2,O3/H2O2/UV) followed the order of H2O2 <UV<03 <O3/H2O2 <O3/H2 O2/UV. The single-factor test of O3/H2O2/UV degradation system showed that higher TCB removal efficiency always found in system with lower initial TCB efficiency or higher ozone transform rate. H2O2 dosage had an optimum value, below or above the optimum value could reduce the TCB removal efficiency. Alkaline condition of O3/H2O2/UV process was in favor to the TCB degradation. The mechanism of TCB degradation in O3/H2O2/UV system was the reaction between TCB and o OH. In the early stages of degradation, the C-Cl bond in benzene rings was attacked by o OH and produced hy-droxylation chlorobenzene

  5. Main: 1H1Y [RPSD[Archive

    Lifescience Database Archive (English)

    Full Text Available 1H1Y イネ Rice Oryza sativa L. D-Ribulose-5-Phosphate 3-Epimerase Oryza Sativa Molecu...V. 326 127 2003 3-Epimerase, Oxidative Pentose Phosphate Pathway, Isomerase SWS:Q9SE42,Q9SE42|EMBL; AF189365; AAF01048.1; -.|PDB; 1H...1Y; X-ray; A/B=1-228.|PDB; 1H1Z; X-ray; A/B=1-228.|Gramene; Q9SE42; -.|GO; GO:001685...ELIQSIKAKGMRPGVSLRPGTPVEEVFPLVEAENPVELVLVMTVEPGFGGQKFMPEMMEKVRALRKKYPSLDIEVDGGLGPSTIDVAASAGANCIVAGSSIFGAAEPGEVISALRKSVEGSQNKS rice_1H1Y.jpg ...

  6. Experimental Study on UV/Mn2+-Fe3+/H2O2 for Wastewater Treatment%UV/Mn2+-Fe3+/H2O2处理染料废水的实验研究

    Institute of Scientific and Technical Information of China (English)

    李明月

    2016-01-01

    研究了常温常压下UV/Mn2+-Fe3+/H2O2光催化非均相反应体系处理偶氮染料模拟废水的特性,并与UV-Mn2+/H2O2、UV/Fe2+/H2O2等体系处理染料废水的效果进行了对比;考察了Mn2+、Fe2+、Fe3+、H2O2投加量对UV/Mn2+-Fe3+/H2O2反应体系处理染料废水的影响.结果表明,UV/Mn2+-Fe3+/H2O2反应体系具有良好的催化氧化作用,在20 w紫外光照射下,100 mg·L-1的直接大红D-GLN在反应20 min时,降解效率高达到90%以上.

  7. Evaluation of a 1-h 75-g oral glucose tolerance test in the diagnosis of gestational diabetes

    Directory of Open Access Journals (Sweden)

    M.A.A. Campos

    2008-08-01

    Full Text Available In order to evaluate the performance of a 1-h 75-g oral glucose tolerance test (OGTT for the diagnosis of gestational diabetes mellitus (GDM, a cohort of 4998 women, 20 years or older, without previous diabetes being treated in prenatal care clinics in Brazil answered a questionnaire and performed a 75-g OGTT including fasting, 1-h and 2-h glucose measurements between their 24th and 28th gestational weeks. Pregnancy outcomes were transcribed from medical registries. GDM was defined according to WHO criteria (fasting: ≥126 mg/dL; 2-h value: ≥140 mg/dL and macrosomia as a birth weight equal to or higher than 4000 g. Areas under the receiver operator characteristic curve (AUC were compared and diagnostic properties of various cut-off points were evaluated. The AUCs for the prediction of macrosomia were 0.606 (0.572-0.637 for the 1-h and 0.589 (0.557-0.622 for the 2-h plasma glucose test. Similar predictability was demonstrable regarding combined adverse outcomes: 0.582 (0.559-0.604 for the 1-h test and 0.572 (0.549-0.595 for the 2-h test. When the 1-h glucose test was evaluated against a diagnosis of GDM defined by the 2-h glucose test, the AUC was 0.903 (0.886-0.919. The cut-off point that maximized sensitivity (83% and specificity (83% was 141 mg/dL, identifying 21% of the women as positive. A cut-off point of 160 mg/dL, with lower sensitivity (62%, had higher specificity (94%, labeling 8.6% as positive. Detection of GDM can be done with a 1-h 75-g OGTT: the value of 160 mg/dL has the same diagnostic performance as the conventional 2-h value (140 mg/dL. The simplification of the test may improve coverage and timing of the diagnosis of GDM.

  8. Theoretical approach of the catalytic hydrochlorination of the 3-amino-2H-1,2,4-triazole

    Directory of Open Access Journals (Sweden)

    Jean Baptiste Mensah

    2009-08-01

    Full Text Available This study was aimed to determine the sites of protonation of the molecule during the hydrochlorination of 3-amino-2H-1,2,4-triazole. The catalytic reaction was carried out on the site MoS3H3+ and on the site ZnCl2. On both catalysts, the reaction led to a selective protonation of the molecule on the same atom of nitrogen of the cycle. But the reaction is endothermic and exothermic on the MoS3H3+ and ZnCl2 catalytic sites, respectively. The calculation method used is Hartree-Fock (HF in the lanl2dz basis set.

  9. Structure of LaH(PO sub 3 H) sub 2. 3H sub 2 O. Structure de LaH(PO sub 3 H) sub 2. 3H sub 2 O

    Energy Technology Data Exchange (ETDEWEB)

    Loukili, M. (Ecole Superieure de Technologie, Fes (Morocco). Dept. Genie Chimique); Durand, J.; Larbot, A.; Cot, L. (Ecole Nationale Superieure de Chimie de Montpellier, 34 (France). Lab. de Physicochimie des Materiaux); Rafiq, M. (Faculte des Sciences, Fes (Morocco). Lab. de Chimie Minerale Appliquee)

    1991-03-15

    Lanthanum hydrogen bis(hydrogenphosphite) trihydrate, LaH(Po{sub 3}H){sub 2}.3H{sub 2}O, M{sub r}=353.8, monoclinic, P2{sub 1}/c, a=9.687 (3), b=7.138 (2), c=13.518 A, {beta}=104.48 (3) deg, V=905.0 (5) A{sup 3}, Z=4, D{sub m}=2.56 (2), D{sub x}=2.598 Mg m{sup -3}, {lambda}(MoK{alpha})=0.71073 A, {mu}(MoK{alpha})=5.103 mm{sup -1}, F(000)=672, T=300 K, R=0.032 for 1018 independent observed reflections. The structure contains two phosphite anions connected by a hydrogen bond. The La{sup 3+} cation is eight coordinated by seven O atoms from phosphite anions and one O atom of a water molecule. (orig.).

  10. H3++H2 isotopic system at low temperatures: Microcanonical model and experimental study

    Science.gov (United States)

    Hugo, Edouard; Asvany, Oskar; Schlemmer, Stephan

    2009-04-01

    State-to-state thermal rate coefficients for reactions of all H3++H2 isotopic variants are derived and compared to new experimental data. The theoretical data are also sought for astrochemical modeling of cold environments (<50K). The rates are calculated on the basis of a microcanonical approach using the Langevin model and the conservation laws of mass, energy, angular momentum, and nuclear spin. Full scrambling of all five nuclei during the collision is assumed for the calculations and alternatively partial dynamical restrictions are considered. The ergodic principle of the collision is employed in two limiting cases, neglecting (weak ergodic limit) or accounting for explicit degeneracies of the reaction mechanisms (strong ergodic limit). The resulting sets of rate coefficients are shown to be consistent with the detailed balance and thermodynamical equilibrium constants. Rate coefficients, k(T ), for the deuteration chain of H3+ with HD as well as H2D+/H3+ equilibrium ratios have been measured in a variable temperature 22-pole ion trap. In particular, the D2H++HD→D3++H2 rate coefficient indicates a change in reaction mechanism when going to higher temperatures. The good overall agreement between experiment and theory encourages the use of the theoretical predictions for astrophysical modeling.

  11. Silver-Catalyzed C(sp(3))-H Chlorination.

    Science.gov (United States)

    Ozawa, Jun; Kanai, Motomu

    2017-03-17

    A silver-catalyzed chlorination of benzylic, tertiary, and secondary C(sp(3))-H bonds was developed. The reaction proceeded with as low as 0.2 mol % catalyst loading at room temperature under air atmosphere with synthetically useful functional group compatibility. The regioselectivity and reactivity tendencies suggest that the chlorination proceeded through a radical pathway, but an intermediate alkylsilver species cannot be ruled out.

  12. 4-Bromo-3-methoxy-1-phenyl-1H-pyrazole

    Directory of Open Access Journals (Sweden)

    Algirdas Šačkus

    2009-11-01

    Full Text Available The title compound was prepared by treatment of 4-bromo-1-phenyl-1H-pyrazol-3-ol with sodium hydride/methyl iodide in good yield. Detailed spectroscopic data (1H NMR, 13C NMR, 15N NMR, IR, MS are presented.

  13. Quantitation of methadone enantiomers in humans using stable isotope-labeled (2H3)-, (2H5)-, and (2H8)Methadone

    Energy Technology Data Exchange (ETDEWEB)

    Nakamura, K.; Hachey, D.L.; Kreek, M.J.; Irving, C.S.; Klein, P.D.

    1982-01-01

    A new technique for simultaneous stereoselective kinetic studies of methadone enantiomers was developed using three deuterium-labeled forms of methadone and GLC-chemical-ionization mass spectrometry. A racemic mixture (1:1) of (R)-(-)-(2H5)methadone (l-form) and (S)-(R)-(2H3)methadone (d-form) was administered orally in place of a single daily dose of unlabeled (+/-)-(2H0)methadone in long-term maintenance patients. Racemic (+/-)-(2H8)methadone was used as an internal standard for the simultaneous quantitation of (2H0)-, (2H3)-, and (2H5)methadone in plasma and urine. A newly developed extraction procedure, using a short, disposable C18 reversed-phase cartridge and improved chemical-ionization procedures employing ammonia gas, resulted in significant reduction of the background impurities contributing to the ions used for isotopic abundance measurements. These improvements enabled the measurement of labeled plasma methadone levels for 120 hr following a single dose. This methodology was applied to the study of methadone kinetics in two patients; in both patients, the analgesically active l-enantiomer of the drug had a longer plasma elimination half-life and a smaller area under the plasma disappearance curve than did the inactive d-form.

  14. Synthesis of 2-Alkenyl-2H-indazoles from 2-(2-Carbonylmethyl)-2H-indazoles.

    Science.gov (United States)

    Lin, Mei-Huey; Liang, Kung-Yu; Tsai, Chang-Hsien; Chen, Yu-Chun; Hsiao, Hung-Chang; Li, Yi-Syuan; Chen, Chung-Hao; Wu, Hau-Chun

    2016-02-19

    A procedure has been developed for synthesis of 2-alkenyl-2H-indazoles starting from 2-(2-carbonylmethyl)-2H-indazoles, which are prepared by gallium/aluminium- and aluminium-mediated, direct, regioselective alkylation of indazoles with α-bromocarbonyl compounds. The structure of 3-(2H-indazol-2-yl)-2H-chromen-2-one was proven by X-ray crystallography. The styrene- and coumarin-2H-indazoles produced by using the new method were found to have interesting fluorescence properties.

  15. 3-[5-(2,4-Dichlorophenyl-1-phenyl-4,5-dihydro-1H-pyrazol-3-yl]-4-hydroxy-2H-chromen-2-one

    Directory of Open Access Journals (Sweden)

    Mohammad Asad

    2011-02-01

    Full Text Available In the title compound, C24H16Cl2N2O3, the chromene ring system is almost planar, with a maximum deviation of 0.042 (1 Å. It makes dihedral angles of 3.72 (6, 73.37 (5 and 12.00 (5° with the dihydropyrazole, benzene and phenyl rings, respectively. An intramolecular O—H...N hydrogen bond forms an S(6 ring motif. In the crystal, molecules are linked via C—H...O interactions, forming an infinite chain along the a axis. The crystal packing is further stabilized by a π–π stacking interaction [centroid–centroid distance = 3.5471 (7 Å] and a Cl...Cl short contact [Cl...Cl = 3.214 (1 Å].

  16. Spin Density Matrix Elements in Exclusive rho^0 Electroproduction on 1H and 2H Targets at 27.5 GeV Beam Energy

    CERN Document Server

    Airapetian, A

    2009-01-01

    Spin Density Matrix Elements (SDMEs) describing the angular distribution of exclusive rho^0 electroproduction and decay are determined in the HERMES experiment with 27.6 GeV beam energy and unpolarized hydrogen and deuterium targets. Eight (fifteen) SDMEs that are related (unrelated) to the longitudinal polarization of the beam are extracted in the kinematic region 1 GeV^2 < Q^2 < 7 GeV^2, 3.0 GeV < W < 6.3 GeV, and -t < 0.4 GeV^2. Within the given experimental uncertainties, a hierarchy of relative sizes of helicity amplitudes is observed. Kinematic dependences of all SDMEs on Q^2 and t are presented, as well as the longitudinal-to-transverse rho^0 electroproduction cross section ratio as a function of Q^2. A small but statistically significant deviation from the hypothesis of s-channel helicity conservation is observed. An indication is seen of a contribution of unnatural-parity-exchange amplitudes; these amplitudes are naturally generated with a quark-exchange mechanism.

  17. (E-4-(5-Hydroxy-2-methylbenzylideneamino-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one

    Directory of Open Access Journals (Sweden)

    Ming-Hua Yang

    2008-10-01

    Full Text Available The title compound, C19H19N3O2, is a Schiff base compound derived from 4-aminoantipyrine and 5-hydroxy-2-methylbenzaldehyde. The molecule adopts a trans configuration about the central C=N bond. There is an intramolecular O—H...N hydrogen bond. Futhermore, weak C—H...O hydrogen bonds lead to the formation of a chain developing parallel to the b axis.

  18. 4-{(E-[2-(4-Iodobutoxybenzylidene]amino}-1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2010-07-01

    Full Text Available The title Schiff base compound, C22H24IN3O2, adopts an E configuration about the central C=N bond. The pyrazolone ring makes a dihedral angle of 49.68 (10° with its attached phenyl ring. The phenolate plane makes dihedral angles of 16.78 (9 and 50.54 (9°, respectively, with the pyrazolone ring and the terminal phenyl ring. An intramolecular C—H...O hydrogen bond generates an S(6 ring motif. In the crystal structure, an intermolecular C—H...O hydrogen bond is also observed.

  19. 1,5-Dimethyl-4-(1-methyl-3-oxo-3-phenylprop-1-enylamino-2-phenyl-1H-pyrazol-3(2H-one

    Directory of Open Access Journals (Sweden)

    Hualing Zhu

    2011-07-01

    Full Text Available In the title compound, C21H21N3O2, an intramolecular N—H...O interaction generates an S(6 ring, which stablizes the enamine–keto tautomer. The S(6 ring makes dihedral angles of 33.07 (7, 56.50 (8 and 38.59 (8°, respectively, with the benzoylacetone benzene ring and the antipyrine pyrazole and benzene rings.

  20. Gas-phase fragmentation of peptides by MALDI in-source decay with limited amide hydrogen (1H/2H) scrambling

    DEFF Research Database (Denmark)

    Bache, Nicolai; Rand, Kasper D; Roepstorff, Peter;

    2008-01-01

    of the gaseous protein (i.e., hydrogen scrambling). Here we investigate the occurrence of scrambling in selectively labeled peptides upon fragmentation by matrix-assisted laser desorption/ionization in-source decay (MALDI ISD). We have utilized peptides with a unique regioselective deuterium incorporation...... that allows us to accurately determine the extent of scrambling upon fragmentation. Our results show that the level of scrambling upon MALDI ISD is so low that the solution deuteration pattern is readily apparent in the gas-phase fragment ions. These results suggest that MALDI ISD may prove useful...

  1. (2E-2-[(2H-1,3-Benzodioxol-5-ylmethylidene]-2,3-dihydro-1H-inden-1-one

    Directory of Open Access Journals (Sweden)

    Abdullah M. Asiri

    2012-04-01

    Full Text Available In the title compound, C17H12O3, each of the five-membered rings in the inden-1-one and 1,3-benzodioxole residues is almost planar (r.m.s. deviations = 0.041 and 0.033 Å, respectively. A small twist about the single bond linking the two residues is evident [the C—C—C—C torsion angle = 8.7 (4°]. Supramolecular zigzag layers propagating in the ac plane are formed in the crystal via C—H...O interactions. The layers are linked via π–π interactions between the five- and six-membered rings of 1,3-benzodioxole residues [centroid–centroid distance = 3.4977 (14 Å].

  2. Eight Zn(II) coordination networks based on flexible 1,4-di(1H-imidazol-1-yl)butane and different dicarboxylates: crystal structures, water clusters, and topologies.

    Science.gov (United States)

    Sun, Di; Xu, Meng-Zhen; Liu, Shan-Shan; Yuan, Shuai; Lu, Hai-Feng; Feng, Sheng-Yu; Sun, Dao-Feng

    2013-09-14

    Eight new Zn(II) coordination polymers based on flexible 1,4-di(1H-imidazol-1-yl)butane and different dicarboxylates, [Zn(dimb)(suc)·2DMF]n (1), [Zn(dimb)(mbda)·3H2O]n (2), [Zn(dimb)(adip)·DMF·2H2O]n (3), [Zn(dimb)(pma)·2.5H2O]n (4), [Zn2(dimb)(tha)2(H2O)]n (5), [Zn(dimb)(chda)·2H2O]n (6), [Zn(dimb)(obda)·DMF]n (7), [Zn(dimb)(tdga)·CH3OH]n (8) (dimb = 1,4-di(1H-imidazol-1-yl)butane, H2suc = succinic acid, H2mbda = m-benzenediacetic acid, H2adip = adipic acid, H2pma = pimelic acid, H2tha = thiophene-2,5-dicarboxylic acid, H2chda = 1,4-cyclohexanedicarboxylic acid, H2obda = o-benzenediacetic acid, H2tdga = thiodiglycolic acid; DMF = N,N'-dimethylformamide), have been synthesized and structurally characterized by single-crystal X-ray diffraction analyses, and further characterized by infrared spectra (IR), elemental analyses, powder X-ray diffractions (PXRD) and thermogravimetric analyses (TGA). Single-crystal X-ray diffraction analysis reveals that 1, 2, 4, 7 and 8 are 2D wavy 4(4)-sql networks with different dimensions of quadrilateral window units, depending on the conformation and length of dimb and dicarboxylates. Complex 3 is a 2D a 6(3)-hcb network incorporating a [Zn2(dimb)2] cyclic subunit. In complex 5, Zn(II) centers as 3-connected node are linked by dimb and tha to form a 3D 8-fold interpenetrating ThSi2 network. Complex 6 is a 4-connected noninterpenetrating cds network. Interestingly, an infinite T4(2)6(2) water tape and a D2h cyclic water tetramer are also found in complexes 2 and 3, respectively. In 1-8, all Zn(II) centers are located in a four-coordinated environment, and dimb and dicarboxylates are 2-connected linkers, but networks with diverse topologies are built, which indicates the linkage of central metal ion, the conformation of dimb and dicarboxylate have important influences on the resulting structures. Furthermore, the solid-state photoluminescence properties of the 1-8 were investigated at 298 and 77 K.

  3. 3-(3,4-Dihydroxyphenyl-8-hydroxy-2H-chromen-2-one

    Directory of Open Access Journals (Sweden)

    Ivan Svinyarov

    2015-10-01

    Full Text Available We report a novel protocol for the synthesis of 3-(3,4-dihydroxyphenyl-8-hydroxy-2H-chromen-2-one via demethylation/delactonization/elimination/lactonization/ decarboxylation domino reaction sequence of diastereomeric mixture of cis- and trans-3-(2,3-dimethoxyphenyl-6,7-dimethoxy-1-oxoisochroman-4-carboxylic acids in boiling HBr/AcOH. The structure of the target compound was established for the first time by means of spectral methods such as 1H-, 13C-, DEPT-135-NMR, IR and HRMS.

  4. Design, synthesis and molecular docking study of thienopyrimidin-4(3H-thiones as antifungal agents

    Directory of Open Access Journals (Sweden)

    Sanjay B. Bari

    2017-01-01

    Full Text Available In an attempt to find a new class of antimicrobial agents, a series of thienopyrimidin-4(3H-thiones 4(H1–H36 were synthesized and evaluated for in vitro antifungal activity against Candida albicans (NCIM 3471, Aspergillus niger (NCIM 545, and Penicillium chrysogenum (NCIM 709. The title compounds were synthesized by thionation of thienopyrimidin-4(3H-ones 3(H1–H36 using Lawesson’s reagent. All the compounds were characterized using elemental analytical (C, H, and N and spectral (FT-IR, 1H NMR, 13C NMR and MS data. Among the tested compounds, 5-(4-chlorophenyl-2-(pyridin-3-ylthieno[2,3-d]pyrimidine-4(3H-thione 4(H11, 2-sulfanyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine-4(3H-thione 4(H18, and 2-(butylsulfanyl-5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidine-4(3H-thione 4(H32 were identified as potentially excellent antifungal agents. They exhibited potent antifungal activity against C. albicans (MIC; 4 μg/mL, A. niger (MIC; 2 μg/mL, and P. chrysogenum (MIC; 2 μg/mL comparable with that of ketoconazole. The binding mode of compounds by SP docking studies shows that it fits well into the active site cavity of DHFR. Lipinski’s rule and in silico ADME pharmacokinetic parameters are within the acceptable range defined for human use thereby indicating their potential as drug-like molecules.

  5. THE ABUNDANCE OF C{sub 3}H{sub 2} AND OTHER SMALL HYDROCARBONS IN THE DIFFUSE INTERSTELLAR MEDIUM

    Energy Technology Data Exchange (ETDEWEB)

    Liszt, Harvey [National Radio Astronomy Observatory, 520 Edgemont Road, Charlottesville, VA 22903-2475 (United States); Sonnentrucker, Paule [Space Telescope Science Institute, 3700 San Martin Drive, Baltimore, MD 21218 (United States); Cordiner, Martin [Astrochemistry Laboratory and the Goddard Center for Astrobiology, Mailstop 691, NASA Goddard Space Flight Center, 8800 Greenbelt Road, Greenbelt, MD 20770 (United States); Gerin, Maryvonne, E-mail: hliszt@nrao.edu [LERMA, UMR 8112 du CNRS, Observatoire de Paris Ecole Normale Superieure, UPMC and UCP (France)

    2012-07-10

    Hydrocarbons are ubiquitous in the interstellar medium, observed in diverse environments ranging from diffuse to molecular dark clouds and strong photon-dominated regions near H II regions. Recently, two broad diffuse interstellar bands (DIBs) at 4881 A and 5450 A were attributed to the linear version of propynylidene l-C{sub 3}H{sub 2}, a species whose more stable cyclic conformer c-C{sub 3}H{sub 2} has been widely observed in the diffuse interstellar medium at radio wavelengths. This attribution has already been criticized on the basis of indirect plausibility arguments because the required column densities are quite large, N(l-C{sub 3}H{sub 2})/E{sub B-V} =4 Multiplication-Sign 10{sup 14} cm{sup -2} mag{sup -1}. Here we present new measurements of N(l-C{sub 3}H{sub 2}) based on simultaneous 18-21 GHz Very Large Array absorption profiles of cyclic and linear C{sub 3}H{sub 2} taken along sight lines toward extragalactic radio-continuum background sources with foreground Galactic reddening E{sub B-V} = 0.1-1.6 mag. We find that N(l-C{sub 3}H{sub 2})/N(c-C{sub 3}H{sub 2}) Almost-Equal-To 1/15-1/40 and N(l-C{sub 3}H{sub 2})/E{sub B-V} Almost-Equal-To (2 {+-} 1) Multiplication-Sign 10{sup 11} cm{sup -2} mag{sup -1}, so that the column densities of l-C{sub 3}H{sub 2} needed to explain the DIBs are some three orders of magnitude higher than what is observed. We also find N(C{sub 4}H)/E{sub B-V} <1.3 Multiplication-Sign 10{sup 13} cm{sup -2} mag{sup -1} and N(C{sub 4}H{sup -})/E{sub B-V} <1 Multiplication-Sign 10{sup 11} cm{sup -2} mag{sup -1} (3{sigma}). Using available data for CH and C{sub 2}H we compare the abundances of small hydrocarbons in diffuse and dark clouds as a guide to their ability to contribute as DIB carriers over a wide range of conditions in the interstellar medium.

  6. 3000m3/h cutter-suction dredge

    Institute of Scientific and Technical Information of China (English)

    2004-01-01

    @@ In October 2004, the Fumin 9 3000 m3/h cutter-suction dredge co-designed by the Dutch IHC and Guangzhou Wenchong Shipyard went through a dock usability test and a 25 meter clean water test. The dredge is the largest of its kind in China, and the most advanced and most efficient cutter-suction dredge in the world. The IHC was responsible for the design of the ship till its working design was taken over by Guangzhou Wenchong Shipyard, the builder of the dredge, who had started its construction on October 23, 2003.

  7. 1,3-Benzothiazole-2(3H)-selone

    OpenAIRE

    Gunay Z. Mammadova; Matsulevich, Zhanna V.; Osmanov, Vladimir K.; Borisov, Alexander V.; Khrustalev, Victor N.

    2011-01-01

    The title compound, C7H5NSSe, is the product of the reaction of 2-chlorobenzothiazole with sodium hydroselenide. The molecule is almost planar (r.m.s. deviation = 0.018 Å) owing to the presence of the long chain of conjugated bonds (Se=C—N—C=C—C=C—C=C). The geometrical parameters correspond well to those of the analog N-methylbenzothiazole-2(3H)-selone, demonstrating that the S atom does not take a significant role in the electron del...

  8. Neurons in the brain of the male cynomolgus monkey accumulate /sup 3/H-medroxyprogesterone acetate (MPA)

    Energy Technology Data Exchange (ETDEWEB)

    Michael, R.P.; Bonsall, R.W.; Rees, H.D.

    1986-03-01

    MPA is a synthetic progestin with androgen-depleting activity. It is used clinically to reduce sexual motivation and aggression in male sex offenders. The mechanisms for its behavioral effects are not known. The authors used steroid autoradiography to help identify sites where MPA may act in the brain of male primates. Twenty-four hours after castration, two adult male cynomolgus macaques, weighing 4.9 and 6.6 kg, were administered 5 mCi /sup 3/H-MPA (NEN, 47.7 Ci/mmol) i.v., and were killed 1 h later. Left sides of the brains and samples of pituitary glands were frozen and 4-micron sections were cut and processed for thaw-mount autoradiography. Radioactivity was concentrated in the nuclei of many neutrons in the ventromedial hypothalamic nucleus (n.), arcuate n., medial preoptic n., and anterior hypothalamic area. Virtually no labeled cells were seen in the bed n. of stria terminalis, lateral septal n., amygdala, or pituitary gland. Right sides of the brains were analyzed by HPLC which demonstrated that 98% of the radioactivity in cell nuclei from the hypothalamus was in the form of unmetabolized /sup 3/H-MPA. The distribution of labelling in the brain following /sup 3/H-MPA administration resembled that previously seen following /sup 3/H-ORG 2058 in female cynomolgus monkeys. These data indicate that MPA has a circumscribed localization in the brain.

  9. Ca2LiC3H: a new complex carbide hydride phase grown in metal flux.

    Science.gov (United States)

    Lang, David A; Zaikina, Julia V; Lovingood, Derek D; Gedris, Thomas E; Latturner, Susan E

    2010-12-15

    The reaction of carbon and CaH2 in a calcium/lithium flux mixture produces crystals of the new compound Ca2LiC3H. This phase forms with a new structure type in tetragonal space group P4/mbm (a = 6.8236(1) Å, c = 3.7518(1) Å, Z = 2, R1 = 0.0151). This is a stuffed variant of the Cs2(NH2)N3 structure, containing hydride anions in octahedral sites; the structure determination by single-crystal X-ray diffraction surprisingly allowed the hydrogen to be detected. The Ca2LiC3H structure also features the rarely seen C3(4-) carbide anion; the protolysis reaction of this compound with ammonium chloride produces C3H4. The electronic properties of Ca2LiC3H were studied by quantum-chemical calculations including band structure and electron localization function (ELF) analysis; the phase is a charge-balanced semiconductor with a calculated band gap of 0.48 eV. This is in agreement with (7)Li, (13)C, and (1)H MAS NMR data, which show resonances in the ionic region instead of the Knight shifted region. ELF analysis of the theoretical nonhydrided Ca2LiC3 structure confirms the ability of these calculations to properly locate hydrides and supports the structural model based on X-ray diffraction data.

  10. Thermal Hydrolysis Synthesis and Characterization of Monoclinic Metahewettite CaV6O16•3H2O

    Institute of Scientific and Technical Information of China (English)

    LI Lanjie; ZHENG Shili; WANG Shaona; DU Hao; ZHANG Yi

    2014-01-01

    Monoclinic metahewettite CaV6O16•3H2O has been fabricated via thermal hydrolysis of calcium vanadate (Ca10V6O25). High purity calcium vanadate precipitate, featuring column structure with surface area of 8.61 m2/g, can be obtained by reacting sodium orthovanadate (Na3VO4) with calcium oxide at 90℃for 2 h. By acidification of calcium vanadate in hot water at pH of 1.0-3.0, the monoclinic metahewettite crystals with uniform particle distribution, layered structure and nonporous structure can be fabricated. With the well crystallized layered structure, CaV6O16•3H2O may be a potential cathode material for secondary batteries as well as super capacitor materials.

  11. The synthesis of Org 3770 labelled with sup 3 H, sup 13 C and sup 14 C. [Antidepressant

    Energy Technology Data Exchange (ETDEWEB)

    Kaspersen, F.M.; Rooij, F.A.M. van; Sperling, E.G.M.; Wieringa, J.H. (Organon International BV, Oss (Netherlands))

    1989-09-01

    The syntheses of 1,2,3,4,10,14b-hexahydro-2-methylpyrazino(2,1-a)pyrido(2,3-c)(2)benazepine (Org 3770) labelled with {sup 3}H (and {sup 2}H), {sup 13}C and {sup 14}C are described. Tritiated Org 3770 was prepared either by exchange under alkaline conditions with tritiated water or catalytic reductive dehalogenation of a chloro analogue with {sup 3}H{sub 2}. {sup 13}C-labelled material was obtained in a seven-step synthesis starting from {sup 13}C-labelled benzene whereas {sup 14}C-Org 3770 was prepared in a three-step synthesis starting with {sup 14}CO{sub 2}. All labelled compounds were analyzed by TLC, HPLC, MS and NMR. (author).

  12. Synthesis and antimicrobial evaluation of 2-(2-butyl- 4-chloro-1H-imidazol-5-yl-methylene-substituted-benzofuran-3-ones

    Directory of Open Access Journals (Sweden)

    Bhaskar S. Dawane

    2010-05-01

    Full Text Available In the present study, the oxidation of 3-(4-chloro-1H-imidazol-5-yl-1-(2-hydroxyphenylprop-2-en-1-ones with mercuric(II acetate in in polyethylene glycol (PEG-400 gave the corresponding 2-((4-chloro-1H-imidazol-5-ylmethylenebenzofuran-3(2H-ones. Newly synthesized compounds were tested for their in vitro antimicrobial activity.

  13. Tissue distribution of 3H-terbutaline in rabbits.

    Science.gov (United States)

    Hsu, C H; Robinson, C P; Basmadjian, G P

    1994-01-01

    Terbutaline is a widely used, selective beta 2-adrenergic agonist whose penetration into brain has not been demonstrated in laboratory animals. Although its tissue uptake has been reported in some animals, no uptake into brain has been demonstrated. A single dose of 20 microCi of 3H-terbutaline along with 10 mg/kg of unlabeled terbutaline was injected into a rabbit marginal ear vein. The distribution of 3H-terbutaline in several tissues was determined 0.5, 1, 3, or 6 hr later. Radioactivity in the brain was well-maintained over the 6 hr observation period. In most tissues, radioactivity peaked in less than 1 hr, then declined. Radioactivity in the urine was high at all time periods and was highest at 3 hr. Thus, terbutaline or a metabolite(s) does cross the blood-brain barrier in rabbits, and the radioactivity in the rabbit brain does not decrease during the 6 hours following terbutaline injection.

  14. Beryllium-induced immune response in C3H mice

    Energy Technology Data Exchange (ETDEWEB)

    Benson, J.M.; Bice, D.E.; Nikula, K.J. [and others

    1995-12-01

    Studies conducted at ITRI over the past several years have investigated whether Beagle dogs, monkeys, and mice are suitable models for human chronic beryllium-induced lung disease (CBD). Recent studies have focused on the histopathological and immunopathological changes occurring in A/J and C3H/HeJ mice acutely exposed by inhalation to Be metal. Lung lesions in both strains of mice included focal lymphocyte aggregates comprised primarily of B lymphocytes and lesser amounts of T-helper lymphocytes and microgranulomas consisting chiefly of macrophages and T-helper lymphocytes. The distribution of proliferating cells within the microgranulomas was similar to the distribution of T-helper cells. These results strongly suggested that A/J and C3H/HeJ mice responded to inhaled Be metal in a fashion similar to humans in terms of pulmonary lesions and the apparent in situ proliferation of T-helper cells. Results of these studies confirm lymphocyte involvement in the pulmonary response to inhaled Be metal.

  15. Evidence for Triangular D_3h Symmetry in 12C

    CERN Document Server

    Marin-Lambarri, D J; Freer, M; Gai, M; Kokalova, Tz; Parker, D J; Wheldon, C

    2014-01-01

    We report a measurement of a new high spin Jp = 5- state at 22.4(0.2) MeV in 12C which fits very well to the predicted (ground state) rotational band of an oblate equilateral triangular spinning top with a D_3h symmetry characterized by the sequence 0+, 2+, 3-, 4+/-, 5- with almost degenerate 4+ and 4- (parity doublet) states. Such a D_3h symmetry was observed in triatomic molecules and it is observed here for the first time in nuclear physics. We discuss a classification of other rotation-vibration bands in 12C such as the (0+) Hoyle band and the (1-) bending mode band and suggest measurements in search of the predicted ("missing") states that may shed new light on clustering in 12C and light nuclei. In particular the observation (or non-observation) of the predicted ("missing") states in the Hoyle band will allow us to conclude the geometrical arrangement of the three alpha-particle composing the Hoyle state at 7.654 MeV in 12C.

  16. Toxicokinetics of ( sup 3 H)microcystin-LR in mice

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, N.A.; Matson, C.F.; Miura, G.A.; Lynch, T.G.; Pace, J.G. (Army Medical Research Inst., Frederick, MD (United States))

    1990-02-26

    Toxicokinetics of ({sup 3}H)microcystin-LR, an algal hepatotoxin, was measured in CD-1 mice (iv, 35 {mu}g/kg, sublethal). The distribution and biological half-lives in plasma were 0.8 and 7 minutes, respectively. Liver rapidly accumulated toxin; uptake half-life was 7 minutes. After 60 minutes, liver, kidney, intestine and carcass retained 67{+-}4, 0.8{+-}0.1, 8.6{+-}0.7 and 6{+-}2% of dose, respectively. By 8 days, 18{+-}1 and 7.6{+-}0.6% of the administered radiolabel appeared in feces and urine, while liver and carcass retained 50{+-}2 and 8{+-}3%, respectively. In urine (6 and 12 hours) and feces (6, 12 and 24 hours) {approximately}60% of the tritium was associated with the parent compound. Hepatic radiolabel was tightly bound to cytosolic protein(s). One hour after injection, 27{+-}3% of the hepatic radiolabel was parent compound and 73{+-}3% was a more-polar component (peak 1). By 8 days, there was a redistribution of hepatic radioactivity: 69{+-}2% with a parent and 4{+-}0.5% with peak 1. The authors conclude that ({sup 3}H)MCYST rapidly accumulated in liver, was metabolized and was associated with cytosolic protein.

  17. The 3H-3He Charge Radii Difference

    Energy Technology Data Exchange (ETDEWEB)

    Myers, Luke S. [Bluffton University, Bluffton, OH; Thomas Jefferson National Accelerator Facility (TJNAF), Newport News, VA (United States); Arrington, John R. [Argonne National Lab. (ANL), Argonne, IL (United States); Higinbotham, Douglas W. [Thomas Jefferson National Accelerator Facility (TJNAF), Newport News, VA (United States)

    2016-03-01

    The upcoming E12-14-009 [1] experiment at Jefferson Lab will determine the ratio of the electric form factors for the A=3 mirror nuclei 3He and 3H. The measurement will use a 1.1 GeV electron beam, a special collimator plate to allow for simultaneous optics measurements, and the low-activity tritium target being prepared for Jefferson Lab. By observing the dependence of the form factor ratio as a function of Q2 over 0.05–0.09 GeV2, the dependence of the radii extraction on the shape of the form factors is minimized. As a result, we anticipate the uncertainty of the extracted charge radii difference to be 0.03 fm, a reduction of 70% from the current measurement. Using precise measurements of the 3He charge radius from isotopic shift or μHe measurements [2–4], we can deduce the absolute 3H charge radius. The results will provide a direct comparison to recent calculations of the charge radii.

  18. Crystal structures of methyl 3-phenyl-4,5-dihydro-1H,3H-benzo[4,5]imidazo[2,1-c][1,4]oxazepine-4-carboxylate and methyl 1-methyl-3-phenyl-4,5-dihydro-1H,3H-benzo[4,5]imidazo[2,1-c][1,4]oxazepine-4-carboxylate

    Directory of Open Access Journals (Sweden)

    J. Govindaraj

    2014-11-01

    Full Text Available The title compounds, C19H18N2O3, (I, and C20H20N2O3, (II, differ only by a methyl substituent on the seven-membered oxazepine ring in (II. In both compounds, these rings have a twist-chair conformation. The phenyl ring makes a dihedral angle of 73.42 (10° with the benzimidazole ring system mean plane (r.m.s. deviation = 0.015 Å in (I and 83.07 (7° in (II (r.m.s. deviation = 0.026 Å. The methyl carboxylate groups are planar to within 0.031 (2 in (I and 0.003 (2 Å in (II. They are inclined to the phenyl and benzimidazole ring system by 33.78 (16 and 87.56 (14°, respectively, in (I and by 53.04 (12 and 60.22 (11°, respectively, in (II. In the crystal of (I, molecules stack in a herringbone fashion and are linked by C—H...O hydrogen bonds, forming chains along [100]. In the crystal of (II, there are no significant intermolecular interactions present.

  19. High pressure oxidation of C2H4/NO mixtures

    DEFF Research Database (Denmark)

    Giménez-López, J.; Alzueta, M.U.; Rasmussen, C.T.

    2011-01-01

    An experimental and kinetic modeling study of the interaction between C2H4 and NO has been performed under flow reactor conditions in the intermediate temperature range (600–900K), high pressure (60bar), and for stoichiometries ranging from reducing to oxidizing conditions. The main reaction...... pathways of the C2H4/O2/NOx conversion, the capacity of C2H4 to remove NO, and the influence of the presence of NOx on the C2H4 oxidation are analyzed. Compared to the C2H4/O2 system, the presence of NOx shifts the onset of reaction 75–150K to lower temperatures. The mechanism of sensitization involves...

  20. Distribution of 3H within purine nucleotides of Ehrlich mouse ascites tumour cells after intraabdominal injection of myo-[2-3H]inositol

    DEFF Research Database (Denmark)

    Christensen, Søren; Klenow, H.; Overgaard-Hansen, Kay

    2000-01-01

    In Ehrlich mouse ascites tumour cells, exposed intra-abdominally to [2-3H]inositol, ATP and GTP presented enough aberrant 3H-label to cause potential interference in the chromatographic analysis of inositol phosphates involved in signal transduction. After acid extraction and charcoal adsorption......% was in ribose and 11% in guanine. This aberrant 3H labelling could be avoided using [1-3H]inositol. Copyright © 2000 John Wiley & Sons, Ltd....

  1. Free radical scavenging potency of quercetin catecholic colonic metabolites: Thermodynamics of 2H(+)/2e(-) processes.

    Science.gov (United States)

    Amić, Ana; Lučić, Bono; Stepanić, Višnja; Marković, Zoran; Marković, Svetlana; Dimitrić Marković, Jasmina M; Amić, Dragan

    2017-03-01

    Reaction energetics of the double (2H(+)/2e(-)), i.e., the first 1H(+)/1e(-) (catechol→ phenoxyl radical) and the second 1H(+)/1e(-) (phenoxyl radical→ quinone) free radical scavenging mechanisms of quercetin and its six colonic catecholic metabolites (caffeic acid, hydrocaffeic acid, homoprotocatechuic acid, protocatechuic acid, 4-methylcatechol, and catechol) were computationally studied using density functional theory, with the aim to estimate the antiradical potency of these molecules. We found that second hydrogen atom transfer (HAT) and second sequential proton loss electron transfer (SPLET) mechanisms are less energy demanding than the first ones indicating 2H(+)/2e(-) processes as inherent to catechol moiety. The Gibbs free energy change for reactions of inactivation of selected free radicals indicate that catecholic colonic metabolites constitute an efficient group of more potent scavengers than quercetin itself, able to deactivate various free radicals, under different biological conditions. They could be responsible for the health benefits associated with regular intake of flavonoid-rich diet.

  2. Bindings of /sup 3/H-prazosin and /sup 3/H-yohimbine to alpha adrenoceptors in the guinea-pig stomach

    Energy Technology Data Exchange (ETDEWEB)

    Taniguchi, T.; Nishikawa, H.

    1988-01-01

    Alpha adrenoceptor subtypes have been investigated by radioligand binding study in guinea-pig stomach using /sup 3/H-prazosin and /sup 3/H-yohimbine. The specific /sup 3/H-prazosin binding to guinea-pig stomach was saturable and of high affinity with a Bmax of 33 fmol/mg protein. Specific /sup 3/H-yohimbine binding to the tissue was also saturable and of high affinity with a Bmax of 150 fmol/mg protein. Adrenergic drugs competed for /sup 3/H-prazosin binding in order of prazosin > phentolamine > methoxamine > norepinephrine > clonidine > epinephrine > yohimbine. These drugs competed for /sup 3/H-yohimbine binding in order of yohimbine > phentolamine > clonidine > epinephrine > norepinephrine > prazosin > methoxamine. They also examined whether dopamine receptors exist in guinea-pig stomach, using radioligand binding study. Specific binding of /sup 3/H-spiperone, /sup 3/H-apomorphine, /sup 3/H-dopamine and /sup 3/H-domperidone was not detectable in the stomach. Dopaminergic drugs such as dopamine, haloperidol, domperidone and sulpiride competed for /sup 3/H-prazosin binding in order of haloperidol > domperidone > dopamine > sulpiride. Metoclopramide, sulpiride and dopamine competed for /sup 3/H-yohimbine binding in order of metoclopramide > sulpiride > dopamine.

  3. Syntheses, structures and characterization of isomorphous Co(II) and Ni(II) coordination polymers based on 2-[(1H-imidazol-1-yl)methyl]-6-methyl-1H-benzimidazole and benzene-1,4-dicarboxylate.

    Science.gov (United States)

    Huang, Qiu Ying; Zhao, Yang; Meng, Xiang Ru

    2017-08-01

    Careful choice of the organic ligands is one of the most important parameters in the rational design and synthesis of coordination polymers. Aromatic polycarboxylates have been widely used in the preparation of metal-organic polymers since they can utilize various coordination modes to form diverse structures and can act as hydrogen-bond acceptors and donors in the assembly of supramolecular structures. Nitrogen-heterocyclic organic compounds have also been used extensively as ligands for the construction of polymers with interesting structures. In the polymers catena-poly[[[diaquabis{2-[(1H-imidazol-1-yl)methyl]-6-methyl-1H-benzimidazole-κN(3)}cobalt(II)]-μ2-benzene-1,4-dicarboxylato-κ(2)O(1):O(4)] dihydrate], {[Co(C8H4O4)(C12H11N4)2(H2O)2]·2H2O}n, (I), and catena-poly[[[diaquabis{2-[(1H-imidazol-1-yl)methyl]-6-methyl-1H-benzimidazole-κN(3)}nickel(II)]-μ2-benzene-1,4-dicarboxylato-κ(2)O(1):O(4)] dihydrate], {[Ni(C8H4O4)(C12H11N4)2(H2O)2]·2H2O}n, (II), the Co(II) or Ni(II) ion lies on an inversion centre and exhibits a slightly distorted octahedral coordination geometry, coordinated by two N atoms from two imidazole rings and four O atoms from two monodentate carboxylate groups and two water molecules. The dicarboxylate ligands bridge metal ions forming a polymeric chain. The 2-[(1H-imidazol-1-yl)methyl]-6-methyl-1H-benzimidazole ligands coordinate to the Co(II) or Ni(II) centres in monodentate modes through an imidazole N atom and are pendant on opposite sides of the main chain. The two structures are isomorphous. In the crystal, the one-dimensional chains are further connected through O-H...O, O-H...N and N-H...O hydrogen bonds, leading to a three-dimensional supramolecular architecture. In addition, the IR spectroscopic properties, PXRD patterns, thermogravimetric behaviours and fluorescence properties of both polymers have been investigated.

  4. Autoradiographie studies of /sup 3/H zearalenone in mice

    Energy Technology Data Exchange (ETDEWEB)

    Appelgren, L.E.; Larsson, P. (Swedish Univ. of Agricultural Sciences, Uppsala. Dept. of Pharmacology); Arora, R.G. (Swedish Univ. of Agriculture, Uppsala. Dept. of Pathology)

    1982-01-01

    Whole body autoradiograms of male, spayed and pregnant female mice after injection of (/sup 3/H) zearalenone showed a rapid excretion of radioactivity into the bile as well as the urine. Specific localization was found in oestrogen target organs as the uterus, interstitial cells of the testicle and the follicles of the ovary. Unlike natural oestrogens zearalenone and/or its metabolites were not found in the adrenal cortex and bronchi of the lungs. Detection of radioactivity in an increased amount of fluid in the pleural and peritoneal cavities suggests an additional site of action of zearalenone. In the pregnant mice used, radioactivity was found only in the foetuses of late pregnancy mainly in the kidney, bile and connective tissue.

  5. Novel Heptamethine 3H-Indocyanines and their Spectral Properties

    Institute of Scientific and Technical Information of China (English)

    Li Qiu WANG; Xiao Jun PENG; Er Hu LU; Jing Nan CUI; Xin Qin GAO

    2005-01-01

    Novel heptamethine 3H-indocyanine dyes are synthesized and embedded into a matrix of silica gel derived from tetraethoxysilicane. The photophysical properties of these near infrared dyes in various solvents and in SiO2 sol gel were investigated. The results show that the dyes containing cyclohexenylene bridge and N-(p-carboxy)benzyl groups have better photostability and longer absorption wavelength than those containing linear heptamethine bridge and/or N-(5-carboxy)pentanyl groups. The absorption maxima of these dyes are in reverse proportion to the polarity of the solvents. The microenvironment of the dyes in SiO2 sol-gel characters medium polarity (between methanol and DMF) according to the absorption maxima.

  6. {sup 1}H MR spectroscopic patterns of normal adult brain

    Energy Technology Data Exchange (ETDEWEB)

    Song, In Chan; Chang, Kee Hyun; Min, Kwan Hong; Kim, Dong Sung; Han, Moon Hee; Kang, Sa Ouk; Min, Byoung Goo; Han, Man Chung [Seoul National Univ. College of Medicine, Seoul (Korea, Republic of)

    1996-10-01

    To evaluate regional differences of {sup 1}H magnetic resonance(MR) spectral patterns in normal adult human brains. A total of 44 {sup 1}H MR spectra in 25 volunteers aged 27-45 were obtained in five regions including the frontal lobe(10), parietal lobe(10), temporal lobe(5), basal ganglia(10) and thalamus(9). {sup 1}H MR spectroscopy(MRS) was performed using a PRESS sequence with a TR of 2000 ms and a TE of 270ms from a volume of cm on a 1.5T clinical MR unit. Relative metabolite ratios of NAA/Cho, NAA/Cr and Cr/Cho in each region were measured and compared. A total of 44 reliable spectra were successfully obtained in all regions. NAA/Cho, NAA/Cr and Cr/Cho ratios varied considerably, ranging from 1.09{+-}0.2 to 2.46{+-}0.25, from 1.72{+-}0.35 to 2.45{+-}0.25 and from 0.64{+-}0.1 to 1.01{+-}0.12, respectively. Significant regional differences in metabolite ratios were observed; higher NAA/Cho and NAA/Cr ratios in the parietal lobe, lower NAA/Cho ratios in the temporal lobe, and lower Cr/Cho ratios in the temporal lobe compared to those of other regions(p<0.05). Differences in metabolite ratios between the right and left frontal lobes, and between the right and left basal ganglias were not significant. {sup 1}H MR spectra of the normal adult human brains using in vivo single voxel {sup 1}H MRS represented significant regional differences in metabolite ratios of NAA/Cho, NAA/Cr and Cr/Cho. Our {sup 1}H MR spectroscopic results are a useful reference for assessing the {sup 1}H MRS pattern of various intracranial diseases.

  7. Following Metabolism in Living Microorganisms by Hyperpolarized (1)H NMR.

    Science.gov (United States)

    Dzien, Piotr; Fages, Anne; Jona, Ghil; Brindle, Kevin M; Schwaiger, Markus; Frydman, Lucio

    2016-09-21

    Dissolution dynamic nuclear polarization (dDNP) is used to enhance the sensitivity of nuclear magnetic resonance (NMR), enabling monitoring of metabolism and specific enzymatic reactions in vivo. dDNP involves rapid sample dissolution and transfer to a spectrometer/scanner for subsequent signal detection. So far, most biologically oriented dDNP studies have relied on hyperpolarizing long-lived nuclear spin species such as (13)C in small molecules. While advantages could also arise from observing hyperpolarized (1)H, short relaxation times limit the utility of prepolarizing this sensitive but fast relaxing nucleus. Recently, it has been reported that (1)H NMR peaks in solution-phase experiments could be hyperpolarized by spontaneous magnetization transfers from bound (13)C nuclei following dDNP. This work demonstrates the potential of this sensitivity-enhancing approach to probe the enzymatic process that could not be suitably resolved by (13)C dDNP MR. Here we measured, in microorganisms, the action of pyruvate decarboxylase (PDC) and pyruvate formate lyase (PFL)-enzymes that catalyze the decarboxylation of pyruvate to form acetaldehyde and formate, respectively. While (13)C NMR did not possess the resolution to distinguish the starting pyruvate precursor from the carbonyl resonances in the resulting products, these processes could be monitored by (1)H NMR at 500 MHz. These observations were possible in both yeast and bacteria in minute-long kinetic measurements where the hyperpolarized (13)C enhanced, via (13)C → (1)H cross-relaxation, the signals of protons binding to the (13)C over the course of enzymatic reactions. In addition to these spontaneous heteronuclear enhancement experiments, single-shot acquisitions based on J-driven (13)C → (1)H polarization transfers were also carried out. These resulted in higher signal enhancements of the (1)H resonances but were not suitable for multishot kinetic studies. The potential of these (1)H-based approaches for

  8. Comparison of (/sup 3/H)pirenzepine and (/sup 3/H)quinuclidinylbenzilate binding to muscarinic cholinergic receptors in rat brain

    Energy Technology Data Exchange (ETDEWEB)

    Luthin, G.R.; Wolfe, B.B.

    1984-03-01

    The properties of (/sup 3/H)quinuclidinylbenzilate ( (/sup 3/H)QNB) binding and (/sup 3/H)pirenzepine ( (/sup 3/H)PZ) binding to various regions of rat brain were compared. (/sup 3/H)PZ appeared to bind with high affinity to a single site, with a Kd value of approximately 15 nM in the cerebral cortex. The rank order of potencies of muscarinic drugs to inhibit binding of either (/sup 3/H)QNB or (/sup 3/H)PZ was QNB greater than atropine . scopolamine greater than pirenzepine greater than oxotremorine greater than bethanechol. Muscarinic antagonists (except PZ) inhibited both (/sup 3/H)PZ and (/sup 3/H)QNB binding with Hill coefficients of approximately 1. PZ inhibited (/sup 3/H)QNB binding in cortex with a Hill coefficient of 0.7, but inhibited (/sup 3/H)PZ binding with a Hill coefficient of 1.0. Hill coefficients for agonists were less than 1. The density of (/sup 3/H)PZ binding sites was approximately half the density of (/sup 3/H)QNB binding sites in cortex, striatum and hippocampus. In pons-medulla and cerebellum, the densities of (/sup 3/H)PZ binding sites were 20 and 0%, respectively, relative to the densities of (/sup 3/H)QNB binding sites. When unlabeled PZ was used to compete for (/sup 3/H)QNB binding, the relative number of high-affinity PZ binding sites in cortex, pons and cerebellum agreed with the relative number of (/sup 3/H)PZ binding sites in those regions. The binding of (/sup 3/H)PZ and (/sup 3/H)QNB was nonadditive in cortex. GTP inhibited high-affinity oxotremorine binding, but not PZ binding. Together, these data suggest that (/sup 3/H)PZ binds to a subset of (/sup 3/H)QNB binding sites. Whether this subset reflects the existence of subtypes of muscarinic receptors or is a consequence of coupling to another membrane protein remains to be seen.

  9. Molecular characterization of barley 3H semi-dwarf genes.

    Directory of Open Access Journals (Sweden)

    Haobing Li

    Full Text Available The barley chromosome 3H accommodates many semi-dwarfing genes. To characterize these genes, the two-rowed semi-dwarf Chinese barley landrace 'TX9425' was crossed with the Australian barley variety 'Franklin' to generate a doubled haploid (DH population, and major QTLs controlling plant height have been identified in our previous study. The major QTL derived from 'TX9425' was targeted to investigate the allelism of the semi-dwarf gene uzu in barley. Twelve sets of near-isogenic lines and a large NILF2 fine mapping population segregating only for the dwarfing gene from 'TX9425' were developed. The semi-dwarfing gene in 'TX9425' was located within a 2.8 cM region close to the centromere on chromosome 3H by fine mapping. Molecular cloning and sequence analyses showed that the 'TX9425'-derived allele contained a single nucleotide substitution from A to G at position 2612 of the HvBRI1 gene. This was apparently the same mutation as that reported in six-rowed uzu barley. Markers co-segregating with the QTL were developed from the sequence of the HvBRI1 gene and were validated in the 'TX9425'/'Franklin' DH population. The other major dwarfing QTL derived from the Franklin variety was distally located on chromosome 3HL and co-segregated with the sdw1 diagnostic marker hv20ox2. A third dwarfing gene, expressed only in winter-sown trials, was identified and located on chromosome 3HS. The effects and interactions of these dwarfing genes under different growing conditions are discussed. These results improve our understanding of the genetic mechanisms controlling semi-dwarf stature in barley and provide diagnostic markers for the selection of semi-dwarfness in barley breeding programs.

  10. Quasifree Lambda, Sigma^0, and Sigma^- electroproduction from 1,2H, 3,4He, and Carbon

    Energy Technology Data Exchange (ETDEWEB)

    F. Dohrmann; A. Ahmidouch; C.S. Armstrong; J. Arrington; R. Asaturyan; S. Avery; K. Bailey; H. Bitao; H. Breuer; D.S. Brown; R. Carlini; J. Cha; N. Chant; E. Christy; A. Cochran; L. Cole; J. Crowder; S. Danagoulian; M. Elaasar; R. Ent; H. Fenker; Y. Fujii; L. Gan; K. Garrow; D.F. Geesaman; P. Gueye; K. Hafidi; W. Hinton; H. Juengst; C. Keppel; Y. Liang; J.H. Liu; A. Lung; D. Mack; P. Markowitz; J. Mitchell; T. Miyoshi; H. Mkrtchyan; S.K. Mtingwa; B. Mueller; G. Niculescu; I. Niculescu; D. Potterveld; B.A. Raue; P.E. Reimer; J. Reinhold; J. Roche; M. Sarsour; Y. Sato; R.E. Segel; A. Semenov; S. Stepanyan; V. Tadevosyan; S. Tajima; L. Tang; A. Uzzle; S. Wood; H. Yamaguchi; C. Yan; L. Yuan; B. Zeidman; M. Zeier; B. Zihlmann

    2007-07-30

    Kaon electroproduction from light nuclei and hydrogen, using 1H, 2H, 3He, 4He, and Carbon targets has been measured at Jefferson Laboratory. The quasifree angular distributions of Lambda and Sigma hyperons were determined at Q^2= 0.35(GeV/c)^2 and W= 1.91GeV. Electroproduction on hydrogen was measured at the same kinematics for reference.

  11. 5-Amino-1H-1,2,4-triazol-4-ium-3-carboxylate hemihydrate

    Directory of Open Access Journals (Sweden)

    José A. Fernandes

    2011-08-01

    Full Text Available The asymmetric unit of the title compound, C3H4N4O2·0.5H2O, comprises two whole molecules of 5-amino-1H-1,2,4-triazole-3-carboxylic acid in its zwitterionic form (proton transfer occurs from the carboxylic acid group to the N heteroatom at position 1, plus one water molecule of crystallization. The organic moieties are disposed into supramolecular layers linked by N—H...O and N—H...N hydrogen bonds parallel to the bc plane. Additional O—H...O and N—H...O hydrogen bonds involving the water molecules and the organic molecules lead to the formation of double-deck supramolecular arrangements which are interconnected along the a axis via π–π stacking [centroid–centroid distance = 3.507 (3 Å].

  12. Synthesis of new 1H-1,2,3-triazole-1,4-naphthoquinones

    Directory of Open Access Journals (Sweden)

    Wagner O. Valença

    2012-06-01

    Full Text Available In this work, were synthesized new 1H-1,2,3-triazole-1,4-naphthoquinones via 1,3-dipolar cycloaddition reaction using CuI/acetonitrile without addition of base or ligand. The compounds (3a-i were obtained in moderate-to-good yields 45-92%. To prepare (3d, we obtain a mixture of (3d and (4 in a ratio 3:1, that it was difficult to separate. The low yield for the compound (3f can be also justified based in the formation of aminonaphthoquinone (4. The acetylation of (3h and (3i afforded the compounds (5 and (6 in 77% and 35% of yields, respectively. The low yield of (6 was due to formation of 35 % of the elimination product (7.

  13. Clinical and treatment effects on /sup 3/H-clonidine and /sup 3/H-imipramine binding in elderly depressed patients

    Energy Technology Data Exchange (ETDEWEB)

    Georgotas, A.; Schweitzer, J.; McCue, R.E.; Armour, M.; Friedhoff, A.J.

    1987-06-01

    /sup 3/H-clonidine and /sup 3/H-imipramine binding were measured in depressed patients, 55 years and older. There was no significant difference in either /sup 3/H-clonidine or /sup 3/H-imipramine binding between depressed patients and age- and sex-matched controls. There was no significant correlation between /sup 3/H-clonidine or /sup 3/H-imipramine binding and severity of depression before treatment. There was a significant negative correlation between the K/sub D/ of /sup 3/H-imipramine binding sites and Hamilton score over seven weeks of antidepressant treatment. There was no significant difference between receptor data of responders and nonresponders to antidepressant treatment. 19 references, 2 tables.

  14. Temperature and pressure dependent rate coefficients for the reaction of C2H4 + HO2 on the C2H4O2H potential energy surface.

    Science.gov (United States)

    Guo, JunJiang; Xu, JiaQi; Li, ZeRong; Tan, NingXin; Li, XiangYuan

    2015-04-02

    The potential energy surface (PES) for reaction C2H4 + HO2 was examined by using the quantum chemical methods. All rates were determined computationally using the CBS-QB3 composite method combined with conventional transition state theory(TST), variational transition-state theory (VTST) and Rice-Ramsberger-Kassel-Marcus/master-equation (RRKM/ME) theory. The geometries optimization and the vibrational frequency analysis of reactants, transition states, and products were performed at the B3LYP/CBSB7 level. The composite CBS-QB3 method was applied for energy calculations. The major product channel of reaction C2H4 + HO2 is the formation C2H4O2H via an OH(···)π complex with 3.7 kcal/mol binding energy which exhibits negative-temperature dependence. We further investigated the reactions related to this complex, which were ignored in previous studies. Thermochemical properties of the species involved in the reactions were determined using the CBS-QB3 method, and enthalpies of formation of species were compared with literature values. The calculated rate constants are in good agreement with those available from literature and given in modified Arrhenius equation form, which are serviceable in combustion modeling of hydrocarbons. Finally, in order to illustrate the effect for low-temperature ignition of our new rate constants, we have implemented them into the existing mechanisms, which can predict ethylene ignition in a shock tube with better performance.

  15. 3,4-Methylenedioxyamphetamine (MDA) analogues exhibit differential effects on synaptosomal release of 3H-dopamine and 3H-5-hydroxytryptamine

    Energy Technology Data Exchange (ETDEWEB)

    McKenna, D.J.; Guan, X.M.; Shulgin, A.T. (Department of Neurology Neurological Sciences, Stanford University Medical Center, CA (USA))

    1991-03-01

    The effect of various analogues of the neurotoxic amphetamine derivative, MDA (3,4-methylenedioxyamphetamine) on carrier-mediated, calcium-independent release of 3H-5-HT and 3H-DA from rat brain synaptosomes was investigated. Both enantiomers of the neurotoxic analogues MDA and MDMA (3,4-methylenedioxymethamphetamine) induce synaptosomal release of 3H-5-HT and 3H-DA in vitro. The release of 3H-5-HT induced by MDMA is partially blocked by 10(-6) M fluoxetine. The (+) enantiomers of both MDA and MDMA are more potent than the (-) enantiomers as releasers of both 3H-5-HT and 3H-DA. Eleven analogues, differing from MDA with respect to the nature and number of ring and/or side chain substituents, also show some activity in the release experiments, and are more potent as releasers of 3H-5-HT than of 3H-DA. The amphetamine derivatives {plus minus}fenfluramine, {plus minus}norfenfluramine, {plus minus}MDE, {plus minus}PCA, and d-methamphetamine are all potent releasers of 3H-5-HT and show varying degrees of activity as 3H-DA releasers. The hallucinogen DOM does not cause significant release of either 3H-monoamine. Possible long-term serotonergic neurotoxicity was assessed by quantifying the density of 5-HT uptake sites in rats treated with multiple doses of selected analogues using 3H-paroxetine to label 5-HT uptake sites. In the neurotoxicity study of the compounds investigated, only (+)MDA caused a significant loss of 5-HT uptake sites in comparison to saline-treated controls. These results are discussed in terms of the apparent structure-activity properties affecting 3H-monoamine release and their possible relevance to neurotoxicity in this series of MDA congeners.

  16. Selective labeling of serotonin uptake sites in rat brain by (/sup 3/H)citalopram contrasted to labeling of multiple sites by (/sup 3/H)imipramine

    Energy Technology Data Exchange (ETDEWEB)

    D' Amato, R.J.; Largent, B.L.; Snowman, A.M.; Snyder, S.H.

    1987-07-01

    Citalopram is a potent and selective inhibitor of neuronal serotonin uptake. In rat brain membranes (/sup 3/H)citalopram demonstrates saturable and reversible binding with a KD of 0.8 nM and a maximal number of binding sites (Bmax) of 570 fmol/mg of protein. The drug specificity for (/sup 3/H)citalopram binding and synaptosomal serotonin uptake are closely correlated. Inhibition of (/sup 3/H)citalopram binding by both serotonin and imipramine is consistent with a competitive interaction in both equilibrium and kinetic analyses. The autoradiographic pattern of (/sup 3/H)citalopram binding sites closely resembles the distribution of serotonin. By contrast, detailed equilibrium-saturation analysis of (/sup 3/H)imipramine binding reveals two binding components, i.e., high affinity (KD = 9 nM, Bmax = 420 fmol/mg of protein) and low affinity (KD = 553 nM, Bmax = 8560 fmol/mg of protein) sites. Specific (/sup 3/H)imipramine binding, defined as the binding inhibited by 100 microM desipramine, is displaced only partially by serotonin. Various studies reveal that the serotonin-sensitive portion of binding corresponds to the high affinity sites of (/sup 3/H)imipramine binding whereas the serotonin-insensitive binding corresponds to the low affinity sites. Lesioning of serotonin neurons with p-chloroamphetamine causes a large decrease in (/sup 3/H)citalopram and serotonin-sensitive (/sup 3/H)imipramine binding with only a small effect on serotonin-insensitive (/sup 3/H)imipramine binding. The dissociation rate of (/sup 3/H)imipramine or (/sup 3/H)citalopram is not altered by citalopram, imipramine or serotonin up to concentrations of 10 microM. The regional distribution of serotonin sensitive (/sup 3/H)imipramine high affinity binding sites closely resembles that of (/sup 3/H)citalopram binding.

  17. Quantitative analysis of norfloxacin by 1H NMR and HPLC.

    Science.gov (United States)

    Frackowiak, Anita; Kokot, Zenon J

    2012-01-01

    1H NMR and developed previously HPLC methods were applied to quantitative determination of norfloxacin in veterinary solution form for pigeon. Changes in concentration can lead to significant changes in the 1H chemical shifts of non-exchangeable aromatic protons as a result of extensive self-association phenomena. This chemical shift variation of protons was analyzed and applied in the quantitative determination of norfloxacin. The method is simple, rapid, precise and accurate, and can be used for quality control of this drug.

  18. Synthesis and Antimicrobial Activity of Some Derivatives on the Basis (7-hydroxy-2-oxo-2H-chromen-4-yl-acetic Acid Hydrazide

    Directory of Open Access Journals (Sweden)

    Elizabeth Has-Schon

    2006-03-01

    Full Text Available (7-Hydroxy-2-oxo-2H-chromen-4-yl-acetic acid hydrazide (2 was prepared from (7-hydroxy-2-oxo-2H-chromen-4-yl-acetic acid ethyl ester (1 and 100% hydrazine hydrate. Compound 2, is the key intermediate for the synthesis of several series of new compounds such as Schiff’s bases 3a-l, formic acid N'-[2-(7-hydroxy-2-oxo-2H- chromen-4-ylacetyl] hydrazide (4, acetic acid N'-[2-(7-hydroxy-2-oxo-2H-chromen-4- yl-acetyl] hydrazide (5, (7-hydroxy-2-oxo-2H-chromen-4-yl-acetic acid N'-[2-(4- hydroxy-2-oxo-2H-chromen-3-yl-2-oxoethyl] hydrazide (6, 4-phenyl-1-(7-hydroxy-2- oxo-2H-chromen- 4-acetyl thiosemicarbazide (7, ethyl 3-{2-[2-(7-hydroxy-2-oxo-2H- chromen-4-yl-acetyl]hydrazono}butanoate (8, (7-hydroxy-2-oxo-2H-chromen-4-yl- acetic acid N'-[(4-trifluoromethylphenyliminomethyl] hydrazide (9 and (7-hydroxy-2- oxo-2H-chromen-4-ylacetic acid N'-[(2,3,4-trifluorophenylimino-methyl] hydrazide (10. Cyclo- condensation of compound 2 with pentane-2,4-dione gave 4-[2-(3,5- dimethyl-1H-pyrazol-1-yl-2-oxoethyl]-7-hydroxy-2H-chromen-2-one (11, while with carbon disulfide it afforded 7-hydroxy-4-[(5-mercapto-1,3,4-oxadiazol-2-ylmethyl]-2H- chromen-2-one (12 and with potassium isothiocyanate it gave 7-hydroxy-4-[(5- mercapto-4H-1,2,4-triazol-3-ylmethyl]-2H-chromen-2-one (14. Compound 7 was cyclized to afford 2-(7-hydroxy-2-oxo-2H-chromen-4-yl-N ́-(4-oxo-2-phenylimino- thiazolidin-3-yl acetamide (15.

  19. Recovery of (/sup 3/H)noradrenaline from different metabolic compartments of rat brain with respect to the role of catechol-O-methyltransferase

    Energy Technology Data Exchange (ETDEWEB)

    Koester, G.; Goede, E.; Breuer, H.

    1984-03-01

    Rats were treated with reserpine, desmethyl-imipramine, or carrier, either alone or in combination with tropolone. Either 10 min (t1) or 1 h (t2) after intraventricular injection of (/sup 3/H)noradrenaline, they were decapitated. The total /sup 3/H activity and the recovery of (/sup 3/H)noradrenaline were determined in tissue extracts from various brain regions. Maximum total /sup 3/H activity was measured at t1 in all tropolone-treated rats; the mean sum of these results served as an estimate of the initial tissue concentration of (/sup 3/H)noradrenaline. At t1, 40-50% of the sum of (/sup 3/H)noradrenaline and its metabolites was recovered unchanged in normal rats; reserpine and DMI reduced the recovery to 18-27%. In all groups, the decline of (/sup 3/H)noradrenaline was retarded after t1. Inhibition of catechol-O-methyltransferase by tropolone caused consistently elevated (/sup 3/H)noradrenaline levels, but did not affect the metabolic rate after t1 when compared with similarly pretreated, but tropolone-free rats. Thus, if catechol-O-methyltransferase was inhibited during the injection of (/sup 3/H)noradrenaline, a higher percentage of the amine had been taken up into spaces with a slow noradrenaline turnover. The maximum increase was seen when the neuronal uptake1 was inhibited by desmethylimipramine. This supported the hypothesis that an additional extraneuronal space exists, in addition to the known intraneuronal and extraneuronal compartments, which has a slow noradrenaline turnover. The tropolone effect on the noradrenaline recovery possibly shows that there might be a saturable ''methylating system,'' similar to that described for the periphery, in which catechol-O-methyltransferase is linked to the extraneuronal uptake.

  20. Theoretical Studies on N2H+O Reaction

    Institute of Scientific and Technical Information of China (English)

    L(U) Ying-wen; L(U) Wen-cai; SU Zhong-min

    2008-01-01

    The N2H+O potential energy profile was studied at the CCSD(T)/6-311G++(dfp)//MP2/6-311G(d,p) level.Reactions associated with four intermediates(cis-HNNO, trans-HNNO, NNHO, and NNOH) were investigated. The results indicate that N2H+O reaction toward H+N2O is more favored than that toward N2+OH, consistent with previous experimental studies. The pathways for the two reactions are found to go through cis-HNNO, transition state, and finally to the products. The N2H+O→NH+NO reaction was studied in detail. Product NO in such a reaction is likely to occur via cis-HNNO, followed by trans-HNNO, and finally dissociates into NH+NO. These results suggest that N2H+O→NH+NO is an important channel in NO production.

  1. PLASMA POLYMERIZATION OF ACETYLENE/CO2/H2

    Institute of Scientific and Technical Information of China (English)

    ZHENG Ji; FANG Yuee; SHI Tianyi; SHOHEI INOUE

    1989-01-01

    A study has been made on the plasma polymerization of acetylene/CO2/H2 in a capacitively coupled RF plasma. The monomer mixture yielded a crosslinked film with light brown color. A kinetic study is reported for the plasma polymerization of acetylene/CO2/H2. The effects of discharge power level and reactor geometry on the rate of polymer formation are reported. The structure of the plasma polymer is investigated by IR study.

  2. Tissue Distribution of [3H]—Nicotine in Rats

    Institute of Scientific and Technical Information of China (English)

    ParimalChowdhury; RyuichiroDOI; 等

    1993-01-01

    This study was conducted in adult male Sprageue-Dawley rats to determine the distribution of [3H]-nicotine in blood and tissues following a bolus injection and a constant infusion of pure nicotine.The animalw were anesthetized and injectd with either 0.5ml of nicotine solution or given a constant infusion of the same nicotine solution with indentical amounts of radioactive nicotine.After sacrifice.blood,brain,trachea,salivery gland, esophagus,lung,heart,liver,fundus,antrum,spleen,pancreas,duodenum,jejunum,ileum, cecum,colon,kidneys,adrenal gland,and testes were collected and measured for radioactivity by scintillation counting.The distribution of nicotine was found highest in kidneys by both routes of administration.Higher accumulations were also found in salivary and adrenal glands,fundus,antrum,duodenum,jejunum,ileum and colon.Retention of nicotine via constant infusion was significantly higher in esophagus,fundus antrum,spleen,cecum, pancreas,testes,heart and muscle when compared with bolus injection,Six-fold increase in retention of blood levels of nicotine were ofund with constant infusion.(P<0.05).The results indicate that longer retention of nicotine occurs in blood and other specific tissues such as esophagus,fundus,antrum,spleen,cecum,pancreas,testes,heart and muscle via constant exposure.These data may implicate the predisposition of these tissues to patologic manifestations.

  3. Diaqua(5-methyl-1H-pyrazole-3-carboxylato(4-nitrobenzoatocopper(II

    Directory of Open Access Journals (Sweden)

    Shan-shan Zhang

    2009-02-01

    Full Text Available In the title complex, [Cu(C7H4NO4(C5H5N2O2(H2O2], the CuII ion is coordinated in a slightly distorted square-pyramidal enviroment. The basal plane is formed by an N atom and an O atom from a 5-methyl-1H-pyrazole-3-carboxylate ligand and by two O atoms from two water ligands. The apical position is occupied by a carboxylate O atom from a 4-nitrobenzoate ligand. In the crystal structure, intermolecular O—H...O and N—H...O hydrogen bonds link complex moleclues, forming extended chains parallel to the a axis.

  4. Metabolite Characterization in Peritoneal Dialysis Effluent Using High-resolution 1H and 1H-13C NMR Spectroscopy

    CERN Document Server

    Guleria, Anupam; Rawat, Atul; Khetrapal, C L; Prasad, Narayan; Kumar, Dinesh

    2014-01-01

    Metabolite analysis of peritoneal dialysis (PD) effluent may provide information regarding onset and progression of complications associated with prolonged PD therapy. In this context, the NMR detectable small metabolites of PD effluent samples were characterized using high resolution 1H and 1H-13C NMR spectroscopy. The various spectra were recorded (at 800 MHz proton frequency) on PD effluent samples obtained after 4 hour (intraperitoneal) dwell time from patients with end stage renal failure (ESRF) and continuing normally on PD therapy. Inspite of devastating spectral feature of PD effluent due to the presence of intense resonances from glucose and lactate, we were able to identify about 53 small endogenous metabolites (including many complex coupled spin systems) and more than 90 % of the total CH cross peaks of 1H-13C HSQC spectrum were identified specific to various metabolites of PD effluent. We foresee that the characteristic fingerprints of various metabolites of control PD effluent samples will be us...

  5. Exploring the dynamics of C/H and C/Cl exchanges in the C(3P) + C2H3Cl reaction

    Science.gov (United States)

    Lee, Shih-Huang; Chen, Wei-Kan; Chin, Chih-Hao; Huang, Wen-Jian

    2013-10-01

    The dynamics of the C(3P) + C2H3Cl reaction at collision energy 3.8 kcal mol-1 was investigated in a crossed molecular-beam apparatus using synchrotron vacuum-ultraviolet ionization. Time-of-flight spectra of products C3H2Cl, C3H3, and Cl were recorded at various laboratory scattering angles, from which translational-energy distributions and angular distributions of product channels C3H2Cl + H and C3H3 + Cl were derived. Cl correlates satisfactorily with C3H3 in linear momentum and angular distributions, which confirms the production of C3H3 + Cl. The H-loss (Cl-loss) channel has average translational-energy release 14.3 (8.8) kcal mol-1 corresponding to a fraction 0.30 (0.14) of available energy into the translational degrees of freedom of product HCCCHCl + H (H2CCCH + Cl). The branching ratio of channel H to channel Cl was determined approximately as 12:88. The measurements of translational-energy releases and photoionization thresholds cannot distinguish HCCCHCl from H2CCCCl because both isomers have similar enthalpy of formation and ionization energy; nevertheless, the Rice-Ramsperger-Kassel-Marcus calculation prefers HCCCHCl. The measurement of photoionization spectra identifies product C3H3 as H2CCCH (propargyl). Both products C3H2Cl + H and C3H3 + Cl might correlate to the same triplet intermediate H2CCCHCl but have distinct angular distributions; the former is nearly isotropic whereas the latter is forward biased. A comparison with the C(3P) + C2H3F reaction is stated.

  6. Nuclear receptor NR1H3 in familial multiple sclerosis

    Science.gov (United States)

    Wang, Zhe; Sadovnick, A. Dessa; Traboulsee, Anthony L.; Ross, Jay P.; Bernales, Cecily Q.; Encarnacion, Mary; Yee, Irene M.; de Lemos, Madonna; Greenwood, Talitha; Lee, Joshua D.; Wright, Galen; Ross, Colin J.; Zhang, Si; Song, Weihong; Vilariño-Güell, Carles

    2016-01-01

    SUMMARY Multiple sclerosis (MS) is an inflammatory disease characterized by myelin loss and neuronal dysfunction. Despite the aggregation observed in some families, pathogenic mutations have remained elusive. In this study we describe the identification of NR1H3 p.Arg415Gln in seven MS patients from two multi-incident families presenting severe and progressive disease, with an average age at onset of 34 years. Additionally, association analysis of common variants in NR1H3 identified rs2279238 conferring a 1.35-fold increased risk of developing progressive MS. The p.Arg415Gln position is highly conserved in orthologs and paralogs, and disrupts NR1H3 heterodimerization and transcriptional activation of target genes. Protein expression analysis revealed that mutant NR1H3 (LXRA) alters gene expression profiles, suggesting a disruption in transcriptional regulation as one of the mechanisms underlying MS pathogenesis. Our study indicates that pharmacological activation of LXRA or its targets may lead to effective treatments for the highly debilitating and currently untreatable progressive phase of MS. PMID:27253448

  7. Advanced oxidation removal of hypophosphite by O3/H2O2 combined with sequential Fe(II) catalytic process.

    Science.gov (United States)

    Zhao, Zilong; Dong, Wenyi; Wang, Hongjie; Chen, Guanhan; Wang, Wei; Liu, Zekun; Gao, Yaguang; Zhou, Beili

    2017-08-01

    Elimination of hypophosphite (HP) was studied as an example of nickel plating effluents treatment by O3/H2O2 and sequential Fe(II) catalytic oxidation process. Performance assessment performed with artificial HP solution by varying initial pH and employing various oxidation processes clearly showed that the O3/H2O2─Fe(II) two-step oxidation process possessed the highest removal efficiency when operating under the same conditions. The effects of O3 dosing, H2O2 concentration, Fe(II) addition and Fe(II) feeding time on the removal efficiency of HP were further evaluated in terms of apparent kinetic rate constant. Under improved conditions (initial HP concentration of 50 mg L(-1), 75 mg L(-1) O3, 1 mL L(-1) H2O2, 150 mg L(-1) Fe(II) and pH 7.0), standard discharge (oxidation treatment favored the improvement of phosphorus removal due to the formation of more metal hydroxides. Moreover, as a comparison with lab-scale Fenton approach, the O3/H2O2─Fe(II) oxidation process had more competitive advantages with respect to applicable pH range, removal efficiency, sludge production as well as economic costs. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Synthesis and antimicrobial activities of 1-(3-benzyl-4-oxo-3H-quinazolin-2-yl-4-(substitutedthiosemicarbazide derivatives

    Directory of Open Access Journals (Sweden)

    Alagarsamy Veerachamy

    2015-01-01

    Full Text Available A series of 1-(3-benzyl-4-oxo-3H-quinazolin-2-yl-4-(substituted thiosemicarbazides (AS1-AS10 were obtained by the reaction of 2-hydrazino- 3-benzyl quinazolin-4(3H-one (6 with different dithiocarbamic acid methyl ester derivatives. The key intermediate 3-benzyl-2-thioxo-2,3-dihydro-1Hquinazolin-4-one (4 was obtained by reacting benzyl amine (1 with carbon disulphide and sodium hydroxide in dimethyl sulphoxide to give sodium dithiocarbamate, which was methylated with dimethyl sulfate to yield the dithiocarbamic acid methyl ester (2 and condensed with methyl anthranilate (3 in ethanol yielded the desired compound (4 via the thiourea intermediate. The SH group of compound (4 was methylated for the favorable nucleophilic displacement reaction with hydrazine hydrate, which afford 2-hydrazino-3- benzyl-3H-quinazolin-4-one (6. The IR, 1H, and 13C NMR spectrum of these compounds showed the presence of peaks due to thiosemicarbazides, carbonyl (C=O, NH and aryl groups. The quinazolin-4-one moiety molecular ion peaks (m/z 144 were observed all the mass spectrum of compounds (AS1-AS10. Elemental (C, H, N analysis satisfactorily confirmed purity of the synthesized compounds and elemental composition. All synthesized compounds were also screened for their antimicrobial activity against selective gram positive and gram negative by agar dilution method. In the present study compounds AS8 and AS9 were emerged as the most active compounds of the series.

  9. Stapled Peptides by Late-Stage C(sp(3) )-H Activation.

    Science.gov (United States)

    Noisier, Anaïs F M; García, Jesús; Ionuţ, Ioana A; Albericio, Fernando

    2017-01-02

    Despite the importance of stapled peptides for drug discovery, only few practical processes to prepare cross-linked peptides have been described; thus the structural diversity of available staple motifs is currently limited. At the same time, C-H activation has emerged as an efficient approach to functionalize complex molecules. Although there are many reports on the C-H functionalization of amino acids, examples of post-synthetic peptide C-H modification are rare and comprise almost only C(sp(2) )-H activation. Herein, we report the development of a palladium-catalyzed late-stage C(sp(3) )-H activation method for peptide stapling, affording an unprecedented hydrocarbon cross-link. This method was first employed to prepare a library of stapled peptides in solution. The compatibility with various amino acids as well as the influence of the size (i,i+3 and i,i+4) and length of the staple were investigated. Finally, a simple solid-phase procedure was also established.

  10. SMA Observations of W3(OH) Complex: Physical and Chemical Differentiation between W3(H$_2$O) and W3(OH)

    CERN Document Server

    Qin, Sheng-Li; Wu, Jingwen; Wu, Yuefang; Liu, Tie; Liu, Ying; Sánchez-Monge, Álvaro

    2015-01-01

    We report on the Submillimeter Array (SMA) observations of molecular lines at 270 GHz toward W3(OH) and W3(H$_2$O) complex. Although previous observations already resolved the W3(H$_2$O) into two or three sub-components, the physical and chemical properties of the two sources are not well constrained. Our SMA observations clearly resolved W3(OH) and W3(H$_2$O) continuum cores. Taking the advantage of the line fitting tool XCLASS, we identified and modeled a rich molecular spectrum in this complex, including multiple CH$_3$CN and CH$_3$OH transitions in both cores. HDO, C$_2$H$_5$CN, O$^{13}$CS, and vibrationally excited lines of HCN, CH$_3$CN, and CH$_3$OCHO were only detected in W3(H$_2$O). We calculate gas temperatures and column densities for both cores. The results show that W3(H$_{2}$O) has higher gas temperatures, and larger column densities than W3(OH) as previously observed, suggesting physical and chemical differences between the two cores. We compare the molecular abundances in W3(H$_2$O) to those i...

  11. Synthesis of 4-(4-Methylsulfonylphenyl)-3-phenyl-2(3H)-thiazole Thione Derivatives as New Potential COX-2 Inhibitors

    Institute of Scientific and Technical Information of China (English)

    EMAMI Saeed; FOROUMADI Alireza

    2006-01-01

    Synthesis of novel 4-(4-methylsulfonylphenyl)-3-phenyl-2(3H)-thiazole thione derivatives with functionalized diarylheterocycle pharmacophore as potential COX-2 inhibitors was described. The title compounds were synthesized by cyclocondensation of corresponding dithiocarbamate and 2-bromo-1-(4-methylsulfonylphenyl)ethanone,followed by dehydration with H2SO4. All of the target compounds were characterized by 1H NMR, IR and mass spectral data.

  12. From {sup 3}H to {sup 195m}Pt

    Energy Technology Data Exchange (ETDEWEB)

    Akaboshi, Mitsuhiko [Kyoto Univ., Kumatori, Osaka (Japan). Research Reactor Inst.

    2000-01-01

    Prof. M. Akaboshi reported his works from 1960 to 1990 ages. He started his studies at the biological using {sup 31}P(n, {gamma}) {sup 32}P. This research determined the direction of his groups researches in order that {sup 31}P(n, {gamma}) {sup 32}P reaction has two sides such as reunion and free of {sup 32}P to the parent compound. A noncatalytic phosphorylation was studied by using {sup 31}P formed from {beta} decay of {sup 31}Si. {sup 32}S from {beta} decay of {sup 32}P easily synthesized Cystein. {sup 14}C, {sup 32}P, {sup 3}H water and {sup 90}Y were used as the {beta}-ray irradiation field. By joint use of {sup 195m}Pt-cisplatin, the lethal mechanisms of new kinds of platinum anticancer agents and platinum compounds to cell were researched by a target dose analysis method developed. Cispaladium from {sup 109}Pd was studied, too. His group studied rare earth metal elements and many results were obtained such as they were concentrated specifically by a kind of organisms and the enrichment patterns were changed by elements. Pteridophytes concentrated them, especially Eu and Tb. Ce (IV) and other elements showed strong hydrolysis activity to phosphoric monoester compounds. The activity was 0.11 umole/umole-Ce(IV).hr{sup -1}at 20degC. But breakage of phosphoric acid ester by Ce(IV) was controlled in the presence of protein-peptides. {sup 141}Ce, {sup 160}Tb and {sup 170}Tm proved that they bonded very fast to only proteins. These results indicated that protein existed in the primitive earth before the rare earth elements. (S.Y.)

  13. Relationship between C2H2 reduction, H2 evolution and 15N2 fixation in root nodules of pea (Pisum sativum)

    DEFF Research Database (Denmark)

    Skøt, Leif

    1983-01-01

    The quantitative relationship between C2H2 reduction, H2 evolution and 15N2 fixation was investigated in excised root nodules from pea plants (Pisum sativum L. cv. Bodil) grown under controlled conditions. The C2H2/N2 conversion factor varied from 3.31 to 5.12 between the 32nd and the 67th day...... after planting. After correction for H2 evolution in air, the factor (C2H2-H2)/N2 decreased to values near the theoretical value 3, or in one case to a value significantly (P H2 production but used...... for N2 reduction, is often stated as the relative efficiency (1-H2/C2H2). This factor varied significantly (P H2 and N2, expressed as the H2/N2 ratio, was independent of plant age, however. This discrepancy and the observation...

  14. Diaquatetrakis(1H-imidazole-κN3magnesium dichloride

    Directory of Open Access Journals (Sweden)

    M. Kayalvizhi

    2013-09-01

    Full Text Available In the title compound, [Mg(C3H3N24(H2O2]Cl2, the MgII cation lies on a crystallographic inversion centre and is coordinated by two water molecules and four N-atom donors from monodentate imidazole ligands, giving a slightly distorted octahedral stereochemistry. In the crystal, water O—H...Cl and imidazole N—H...Cl hydrogen bonds give rise to a three-dimensional structure.

  15. Light microscopic autoradiographic localization of (/sup 3/H)pirenzepine and (/sup 3/H)(/sup -/)quinuclidinyl benzilate binding in human stellate ganglia

    Energy Technology Data Exchange (ETDEWEB)

    Yamamura, H.I.; Watson, M.; Wamsley, J.K.; Johnson, P.C.; Roeske, W.R.

    1984-08-13

    The LKB Ultrofilm method of autoradiography has been utilized to anatomically localize putative M/sub 1/ and M/sub 2/ muscarinic receptor subtypes in human stellate ganglia. Ten micron sections were labeled in vitro with either 1 nM of the classical antagonist (/sup 3/H)(/sup -/)quinuclidinyl benzilate ((/sup 3/H)(/sup -/)QNB) or 20 nM of the non-classical antagonist (/sup 3/H)pirenzepine ((/sup 3/H)PZ), using 1 ..mu..M atropine sulfate to define non-specific binding for both ligands. The results indicate that (/sup 3/H)(/sup -/)QNB and (/sup 3/H)PZ binding sites are distributed within the principal ganglion cells and nerve bundles.

  16. Radioactive contamination of the marine environment: Uptake and distribution of3H in Dunaliella bioculata

    Science.gov (United States)

    Strack, S.; Bonotto, S.; Kirchmann, R.

    1980-03-01

    The marine flagellate Dunaliella bioculata, which is easily cultivated under laboratory conditions, is a suitable organism for assessing the importance of the radioactive contamination by3H bound to organic molecules. We have studied the uptake of the following tritiated precursors: thymidine-methyl-3H, adenine-2-3H, uridine-5-3H, l-leucine-4-3H, glycine-2-3H, l-arginine-3.4-3H, 1-aspartic acid-2. 3-3H, 1-phenylalanine-2.3-3H, D-glucose-2-3H and D-glucose-6-3H. Under the experimental conditions (2000 lux; incubation time 30 min), all tritiated molecules are taken up by D. bioculata. Their intracellular concentration may reach that of the external medium. However, leucine and adenine accumulate in the algae: their respective concentrations are 10 and 100 times higher than in the culture medium. The molecular distribution of3H has been studied by various biochemical techniques and by sieve chromatography on sepharose 4B. It has been found that more l-leucine-4-3H is incorporated into acid and acetone soluble substances than into proteins. Adenine-2-3H is mainly incorporated into macromolecules of biological significance (RNA, DNA). CsCl gradient centrifugation has shown that the total DNA of Dunaliella is constituted by a major (ϖ=1.707 g/cm3) and by a minor (ϖ=1.693 g/cm3) component.

  17. Synthesis, structure and NMR characterization of a new monomeric aluminophosphate [ dl-Co(en) 3] 2[Al(HPO 4) 2(H 1.5PO 4) 2(H 2PO 4) 2](H 3PO 4) 4 containing four different types of monophosphates

    Science.gov (United States)

    Chen, Peng; Li, Jiyang; Xu, Jun; Duan, Fangzheng; Deng, Feng; Xu, Ruren

    2009-03-01

    A new zero-dimensional (0D) aluminophosphate monomer [ dl-Co(en) 3] 2[Al(HPO 4) 2(H 1.5PO 4) 2(H 2PO 4) 2](H 3PO 4) 4 (designated AlPO-CJ38) with Al/P ratio of 1/6 has been solvothermally prepared by using racemic cobalt complex dl-Co(en) 3Cl 3 as the template. The Al atom is octahedrally linked to six P atoms via bridging oxygen atoms, forming a unique [Al(HPO 4) 2(H 1.5PO 4) 2(H 2PO 4) 2] 6- monomer. Notably, there exists intramolecular symmetrical O⋯H⋯O bonds, which results in pseudo-4-rings stabilized by the strong H-bonding interactions. The structure is also featured by the existence of four different types of monophosphates that have been confirmed by 31P NMR and 1H NMR spectra. The crystal data are as follows: AlPO-CJ38, [ dl-Co(en) 3] 2[Al(HPO 4) 2(H 1.5PO 4) 2(H 2PO 4) 2](H 3PO 4) 4, M = 1476.33, monoclinic, C2/ c (No. 15), a = 36.028(7) Å, b = 8.9877(18) Å, c = 16.006(3) Å, β = 100.68(3)°, U = 5093.2(18) Å 3,Z = 4, R1 = 0.0509 ( I > 2 σ( I)) and wR2 = 0.1074 (all data). CCDC number 689491.

  18. Antifungal properties of wheat histones (H1-H4) and purified wheat histone H1.

    Science.gov (United States)

    De Lucca, Anthony J; Heden, Lars-Olof; Ingber, Bruce; Bhatnagar, Deepak

    2011-07-13

    Wheat ( Triticum spp.) histones H1, H2, H3, and H4 were extracted, and H1 was further purified. The effect of these histones on specific fungi that may or may not be pathogenic to wheat was determined. These fungi included Aspergillus flavus , Aspergillus fumigatus , Aspergillus niger , Fusarium oxysporum , Fusarium verticillioides , Fusarium solani , Fusarium graminearum , Penicillium digitatum , Penicillium italicum , and Greeneria uvicola . Non-germinated and germinating conidia of these fungi were bioassayed separately. The non-germinated and germinating conidia of all Fusarium species were highly susceptible to the mixture (H1-H4) as well as pure H1, with viability losses of 99-100% found to be significant (p histone mixture and pure H1. F. graminearum was the most sensitive to histone activity. The histones were inactive against all of the non-germinated Penicillium spp. conidia. However, they significantly reduced the viability of the germinating conidia of the Penicillium spp. conidia, with 95% loss at 2.5 μM. Non-germinated and germinating conidia viability of the Aspergillus spp. and G. uvicola were unaffected when exposed to histones up to 10 μM. Results indicate that Fusarium spp. pathogenic to wheat are susceptible to wheat histones, indicating that these proteins may be a resistance mechanism in wheat against fungal infection.

  19. Parkinson's disease: decreased density of /sup 3/H-imipramine and /sup 3/H-paroxetine binding sites in putamen

    Energy Technology Data Exchange (ETDEWEB)

    Raisman, R.; Cash, R.; Agid, Y.

    1986-04-01

    The density of high-affinity /sup 3/H-imipramine and /sup 3/H-paroxetine binding sites (two serotonin-uptake blockers) was decreased in the putamen of parkinsonian patients. The correlation between serotonin levels and the number of /sup 3/H-imipramine and /sup 3/H-paroxetine binding sites suggests that they are located on serotoninergic nerve terminals and could be used to study serotoninergic innervation in the human brain. Since imipramine and paroxetine are powerful antidepressants, these results furthermore suggest that decreased serotoninergic transmission may be implicated in the pathophysiology of depression in Parkinson's disease.

  20. Synthesis of 1-aryl-3-(3,4-dihydro-2H-chromen-5-yl)ureas as TNF-α inhibitors

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A new series of compounds, 1-aryl-3-(3,4-dihydro-2H-chromen-5-yl) ureas, have been synthesized and their structures were confirmed by FAB-MS and 1H NMR. The preliminary pharmacological screening showed that these compounds inhibited TNF-αproduction in lipopolysaccharide (LPS)-stimulated THP-1 cells.

  1. Co(III)-Carbene Radical Approach to Substituted 1H-Indenes.

    Science.gov (United States)

    Das, Braja Gopal; Chirila, Andrei; Tromp, Moniek; Reek, Joost N H; Bruin, Bas de

    2016-07-20

    A new strategy for the catalytic synthesis of substituted 1H-indenes via metalloradical activation of o-cinnamyl N-tosyl hydrazones is presented, taking advantage of the intrinsic reactivity of a Co(III) carbene radical intermediate. The reaction uses readily available starting materials and is operationally simple, thus representing a practical method for the construction of functionalized 1H-indene derivatives. The cheap and easy to prepare low spin cobalt(II) complex [Co(II)(MeTAA)] (MeTAA = tetramethyltetraaza[14]annulene) proved to be the most active catalyst among those investigated, which demonstrates catalytic carbene radical reactivity for a nonporphyrin cobalt(II) complex, and for the first time catalytic activity of [Co(II)(MeTAA)] in general. The methodology has been successfully applied to a broad range of substrates, producing 1H-indenes in good to excellent yields. The metallo-radical catalyzed indene synthesis in this paper represents a unique example of a net (formal) intramolecular carbene insertion reaction into a vinylic C(sp(2))-H bond, made possible by a controlled radical ring-closure process of the carbene radical intermediate involved. The mechanism was investigated computationally, and the results were confirmed by a series of supporting experimental reactions. Density functional theory calculations reveal a stepwise process involving activation of the diazo compound leading to formation of a Co(III)-carbene radical, followed by radical ring-closure to produce an indanyl/benzyl radical intermediate. Subsequent indene product elimination involving a 1,2-hydrogen transfer step regenerates the catalyst. Trapping experiments using 2,2,6,6-tetra-methylpiperidine-1-oxyl (TEMPO) radical or dibenzoylperoxide (DBPO) confirm the involvement of cobalt(III) carbene radical intermediates. Electron paramagnetic resonance spectroscopic spin-trapping experiments using phenyl N-tert-butylnitrone (PBN) reveal the radical nature of the reaction.

  2. Triaquabis(1H-imidazolebis[μ2-2-(oxaloaminobenzoato(3−]dicopper(IIcalcium(II heptahydrate

    Directory of Open Access Journals (Sweden)

    Peng Zhang

    2008-02-01

    Full Text Available In the title heterotrinuclear coordination compound, [CaCu2(C9H4NO52(C3H4N22(H2O3]·7H2O, the Ca2+ cation is in a pentagonal–bipyramidal geometry and bridges two (1H-imidazole[2-(oxaloaminobenzoato(3−]copper(II units in its equatorial plane. Each CuII atom has a normal square-planar geometry. The molecule has approximate local (non-crystallographic mirror symmetry and 23 classical hydrogen bonds are found in the crystal structure.

  3. Analysis list: Zc3h11a [Chip-atlas[Archive

    Lifescience Database Archive (English)

    Full Text Available Zc3h11a Blood,Pluripotent stem cell + mm9 http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Zc3...h11a.1.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/target/Zc3h11a.5.tsv http://dbarch...ive.biosciencedbc.jp/kyushu-u/mm9/target/Zc3h11a.10.tsv http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Zc3...h11a.Blood.tsv,http://dbarchive.biosciencedbc.jp/kyushu-u/mm9/colo/Zc3h11a.Plu

  4. Three new energetic complexes with N,N-bis(1H-tetrazole-5-yl)-amine as high energy density materials: syntheses, structures, characterization and effects on the thermal decomposition of RDX.

    Science.gov (United States)

    Yang, Qi; Song, Xiaxia; Zhang, Wendou; Hou, Lei; Gong, Qibing; Xie, Gang; Wei, Qing; Chen, Sanping; Gao, Shengli

    2017-02-21

    Three new energetic complexes, [Pb(bta)(H2O)]n (1), [PbCu(bta)2(H2O)5]·2H2O (2) and PbCu(bta)2 (3) (H2bta = N,N-bis(1H-tetrazole-5-yl)-amine), have been synthesized and characterised. In particular, 3 was readily synthesized by dehydration of 2 at 190 °C. Single crystal X-ray diffraction revealed that 1 has a 3D framework structure and 2 presents a 3D supermolecular architecture. Thermoanalyses demonstrated that the main frames of 1 and 2 have good thermostabilities up to 314 °C for 1 and 231 °C for 2. Non-isothermal kinetic and thermodynamic parameters of exothermic decomposition processes of 1 and 2 were obtained by Kissinger's and Ozawa's methods. Based on the constant-volume combustion energies measured by a precise rotating-bomb calorimeter, the standard molar enthalpies of formation of 1 and 2 were determined. The calculation of the detonation properties of 1 and 2 and the impact sensitivity tests of 1, 2 and 3 were carried out. In addition, 1, 2 and 3 were explored as combustion promoters to accelerate the thermal decompositions of RDX (1,3,5-trinitro-1,3,5-triazine) by differential scanning calorimetry. Experimental results showed that 1, 2 and 3 can be used as HEDMs in the field of combustion promoters and insensitive 2 can be regarded as a safer form for mass storage and transportation than sensitive 3.

  5. 1H NMR Studies of MgH2

    Science.gov (United States)

    Itoh, Yutaka; Kado, Ryoichi

    We report on 1H NMR studies of commercially available powder MgH2 exposed to air and maybe humidity, which has been believed to be a promising material for hydrogen storage. The Fourier transform of the free-induction decay of the protons indicatesd superposition of broad and narrow components in the NMR spectrum, while the Fourier transform of the 1H nuclear spin-echo reproduced the narrow component. With cooling down below room temperature, the ratio of the narrow peak to the broad spectrum decreased. The broad spectrum is associated with direct dipolar coupled protons on an inhomogeneous rigid lattice. The narrow peak is associated with interstitial protons with more inhomogeneous surroundings.

  6. 5-Pentyl-4-phenylsulfonyl-1H-pyrazol-3-ol

    Directory of Open Access Journals (Sweden)

    Tara Shahani

    2010-06-01

    Full Text Available In the title compound, C14H18N2O3S, the 1H-pyrazole ring is approximately planar, with a maximum deviation of 0.005 (1 Å. The dihedral angle formed between the 1H-pyrazole and phenyl rings is 79.09 (5°. Pairs of intermolecular N—H...O and O...H...N hydrogen bonds form dimers between neighboring molecules, generating R22(10 ring motifs. These dimers are further linked byintermolecular N—H...O and O—H...N hydrogen bonds into a two-dimensional array parallel to the ac plane. The crystal structure is also stabilized by C—H...π interactions.

  7. N-(5-Amino-1H-tetrazol-1-ylformamide

    Directory of Open Access Journals (Sweden)

    Chun-Lin He

    2009-11-01

    Full Text Available In the title compound, C2H4N6O, the planar [maximum deviation = 0.006 (2 Å] aminotetrazole group makes a dihedral angle of 83.65 (8° with the formamide unit. In the crystal structure, intermolecular N—H...N, N—H...O and C—H...N hydrogen bonds are responsible for the formation of a three-dimensional network.

  8. Therapeutic potential of CAMPATH-1H in skeletal tumours

    OpenAIRE

    Fritsche, Raphaela; Grützkau, Andreas; Noske, Aurelia; Melcher, Ingo; Schaser, Klaus-Dieter; Schlag, Peter M.; Kasper, Hans U; Krenn, Veit Jonas; Sers, Christine

    2010-01-01

    Abstract Aim: CD52 is a GPI-anchored glycoprotein that is expressed abundantly on all lymphocytes, monocytes, macrophages, eosinophils and in the male genital tract. To date, the physiological role of CD52 on lymphocytes has not been elucidated. However, an antibody directed to CD52 called CAMPATH-1H has been shown to be capable of depleting lymphocytes. Tissue and cell lines of non-neoplastic bone, cartilage and skeletal tumours were analysed for CD52 expression. Methods and resul...

  9. 7-Iodo-1H-indole-3-carbonitrile

    Directory of Open Access Journals (Sweden)

    Rosanna Meine

    2015-10-01

    Full Text Available The title compound was prepared by a Friedel–Crafts acylation-oxime synthesis-decarboxylation/dehydration sequence starting from commercially available 7-iodoindole with 2-(7-iodo-1H-indol-3-yl-2-oxoacetic acid as isolated intermediate. The structural identity of the title compound was proven by elemental analysis and spectroscopic methods (IR, NMR, EI-MS, and purity was assessed by two independent HPLC methods.

  10. 1-Propyl-1H-indole-2,3-dione

    Directory of Open Access Journals (Sweden)

    Fatima Zahrae Qachchachi

    2016-04-01

    Full Text Available In the title compound, C11H11NO2, the 1H-indole-2,3-dione unit is essentially planar, with an r.m.s. deviation of 0.0387 (13 Å. This plane makes a dihedral angle of 72.19 (17° with the plane of the propyl substituent. In the crystal, chains propagating along the b axis are formed through C—H...O hydrogen bonds.

  11. Quantitative produced water analysis using mobile 1H NMR

    Science.gov (United States)

    Wagner, Lisabeth; Kalli, Chris; Fridjonsson, Einar O.; May, Eric F.; Stanwix, Paul L.; Graham, Brendan F.; Carroll, Matthew R. J.; Johns, Michael L.

    2016-10-01

    Measurement of oil contamination of produced water is required in the oil and gas industry to the (ppm) level prior to discharge in order to meet typical environmental legislative requirements. Here we present the use of compact, mobile 1H nuclear magnetic resonance (NMR) spectroscopy, in combination with solid phase extraction (SPE), to meet this metrology need. The NMR hardware employed featured a sufficiently homogeneous magnetic field, such that chemical shift differences could be used to unambiguously differentiate, and hence quantitatively detect, the required oil and solvent NMR signals. A solvent system consisting of 1% v/v chloroform in tetrachloroethylene was deployed, this provided a comparable 1H NMR signal intensity for the oil and the solvent (chloroform) and hence an internal reference 1H signal from the chloroform resulting in the measurement being effectively self-calibrating. The measurement process was applied to water contaminated with hexane or crude oil over the range 1-30 ppm. The results were validated against known solubility limits as well as infrared analysis and gas chromatography.

  12. DNA Mismatch Repair Interacts with CAF-1- and ASF1A-H3-H4-dependent Histone (H3-H4)2 Tetramer Deposition.

    Science.gov (United States)

    Rodriges Blanko, Elena; Kadyrova, Lyudmila Y; Kadyrov, Farid A

    2016-04-22

    DNA mismatch repair (MMR) is required for the maintenance of genome stability and protection of humans from several types of cancer. Human MMR occurs in the chromatin environment, but little is known about the interactions between MMR and the chromatin environment. Previous research has suggested that MMR coincides with replication-coupled assembly of the newly synthesized DNA into nucleosomes. The first step in replication-coupled nucleosome assembly is CAF-1-dependent histone (H3-H4)2 tetramer deposition, a process that involves ASF1A-H3-H4 complex. In this work we used reconstituted human systems to investigate interactions between MMR and CAF-1- and ASF1A-H3-H4-dependent histone (H3-H4)2 tetramer deposition. We have found that MutSα inhibits CAF-1- and ASF1A-H3-H4-dependent packaging of a DNA mismatch into a tetrasome. This finding supports the idea that MMR occurs before the DNA mismatch is packaged into the tetrasome. Our experiments have also revealed that CAF-1- and ASF1A-H3-H4-dependent deposition of the histone (H3-H4)2 tetramers does not interfere with MMR reactions. In addition, we have established that unnecessary degradation of the discontinuous strand that takes place in both DNA polymerase δ (Pol δ)- and DNA polymerase ϵ (Pol ϵ)-dependent MMR reactions is suppressed by CAF-1- and ASF1A-H3-H4-dependent deposition of the histone (H3-H4)2 tetramers. These data suggest that CAF-1- and ASF1A-H3-H4-dependent deposition of the histone (H3-H4)2 tetramers is compatible with MMR and protects the discontinuous daughter strand from unnecessary degradation by MMR machinery.

  13. Distribution of 3H within purine nucleotides of Ehrlich mouse ascites tumour cells after intraabdominal injection of myo-[2-3H]inositol

    DEFF Research Database (Denmark)

    Christensen, Søren; Klenow, H.; Overgaard-Hansen, Kay

    2000-01-01

    In Ehrlich mouse ascites tumour cells, exposed intra-abdominally to [2-3H]inositol, ATP and GTP presented enough aberrant 3H-label to cause potential interference in the chromatographic analysis of inositol phosphates involved in signal transduction. After acid extraction and charcoal adsorption...

  14. Bis{μ-1-[(2-ethyl-1H-imidazol-1-ylmethyl]-1H-benzotriazole}bis(iodidocadmium

    Directory of Open Access Journals (Sweden)

    Xia Wang

    2011-07-01

    Full Text Available The dinuclear title complex, [Cd2I4(C12H13N52], lies on a crystallographic center of inversion. The CdII atom is four-coordinated by two N atoms from two 1-[(2-ethyl-1H-imidazol-1-ylmethyl]-1H-benzotriazole (bmei ligands and two terminal I atoms in a distorted tetrahedral coordination environment. The CdII atoms are connected to each other by two bridging bmei ligands. The benzotriazole rings in adjacent molecules are almost parallel, with an average interplanar distance of 3.3400 (2 Å and a centroid–centroid distance of 4.852 (2 Å.

  15. Effects of surgical and chemical lesions on striatal (/sup 3/H)threo-(+-)-methylphenidate binding: correlation with (/sup 3/H)dopamine uptake

    Energy Technology Data Exchange (ETDEWEB)

    Janowsky, A.; Berger, P.; Long, R.; Paul, S.M. (National Inst. of Mental Health, Bethesda, MD (USA)); Schweri, M.M.; Skolnick, P. (National Institutes of Health, Bethesda, MD (USA))

    1985-01-22

    The specific binding of (/sup 3/H)threo-(+-)-methylphenidate to membranes prepared from rat striatum was significantly reduced following either surgical lesions of the medial forebrain bundle or intracerebroventricular administration of 6-hydroxydopamine. The decrease in the density of (/sup 3/H)threo-(+-)-methylphenidate binding sites in striatum following chemical or surgical denervation was highly correlated with the decrease in (/sup 3/H)dopamine uptake. In contrast, intracerebroventricular administration of 5,7-dihydroxytryptamine, AF64A, or chronic parenteral administration of reserpine did not alter either the number or apparent affinity of (/sup 3/H)threo-(+-)-methylphenidate binding sites. These data suggest that the specific binding sites for (/sup 3/H)threo-(+-)-methylphenidate in striatum are localized to dopaminergic nerve terminals, and may be associated with the dopamine transport complex.

  16. The distribution and abundance of interstellar C2H

    Science.gov (United States)

    Huggins, P. J.; Carlson, W. J.; Kinney, A. L.

    1984-01-01

    C2H(N = 1-0) emission has been extensively observed in a variety of molecular clouds, including: 12 hot, dense, cloud cores, 3 bright-rimmed clouds (in NGC 1977, IC 1396, and IC 1848), and across the extended OMC - 1 cloud. It has also been observed in the circumstellar envelopes IRC + 10216 and AFGL 2688. Abundance analyses of the molecular clouds yield C2H/(C-13)O abundance ratios of about 0.01, with little variation (less than about a factor of 4) either between clouds or across individual clouds. In the Orion plateau source, the C2H abundance is enhanced by less than a factor of 4, relative to the extended cloud. The generally high levels of C2H found in the molecular clouds are not readily accounted for by simple, steady-state chemical models, and suggest, as do earlier observations of atomic carbon, that the carbon chemistry in dense clouds is more active than is commonly assumed.

  17. Synthesis of 2H-Chromenones from Salicylaldehydes and Arylacetonitriles

    Directory of Open Access Journals (Sweden)

    Chengcai Li

    2017-07-01

    Full Text Available An efficient and convenient protocol for the synthesis of 2H-chromenones has been developed. In the presence of tBuOK in DMF, good to excellent yields of various chromenones were obtained from the corresponding salicylaldehydes and arylacetonitriles. No protection of inert gas atmosphere is required here.

  18. (2S*-2-Ammonio-3-(1H-indol-3-ylpropionate pyridine-2,4-dicarboxylic acid ethanol solvate

    Directory of Open Access Journals (Sweden)

    Kai Di

    2010-05-01

    Full Text Available In the title compound, C11H12N2O2·C7H5NO4·C2H6O, the (2S*-2-amino-3-(1H-indol-3-ylpropionic acid is present in the zwitterionic form. In the crystal structure, 2-amino-3-(1H-indol-3-ylpropionic acid molecules and pyridine-2,4-dicarboxylic acid molecules are linked through strong intermolecular O—H...O and N—H...O hydrogen bonds, forming layers parallel to (100. The layers are linked through the ethanol molecules via somewhat weaker intermolecular O—H...O and N—H...O hydrogen bonds, forming thus a three-dimensional network. Weak C—H...O and N—H...N hydrogen bonding and π–π interactions between the aromatic rings are also present.

  19. High-frequency observations of δ2H and δ18O in storm rainfall

    Science.gov (United States)

    Stoecker, F.; Klaus, J.; Pangle, L. A.; Garland, C.; McDonnell, J. J.

    2012-12-01

    Stable isotopes ratios of hydrogen (2H/1H) and oxygen (18O/16O) are indispensable tools for investigation of the hydrologic cycle. Recent technological advances with laser spectroscopy now enable high-frequency measurement of key water cycle components. While the controls on rainfall isotope composition have been known generally for some time, our understanding of the effect of inter- and intra-storm processes on fine scale rainfall isotope composition is poorly understood. Here we present a new approach to observe inter- and intra-storm isotope variability in precipitation in high-frequency. We investigate the temporal development of δ2H and δ18O within and between discrete rainstorm. δ2H and δ18O in precipitation was measured from November 2011 to February 2012 in Corvallis, OR using a flow-cell combined with a Liquid Water Isotope Analyzer (LWIA-24d, Los Gatos Research, Inc.). The average sample frequency was 15 samples per hour, resulting in more than 3100 samples during the observation period. 27 separate rainstorms were identified in the dataset based on minimum inter-event time, minimum precipitation depth, and minimum number of isotope measurements. Event meteoric water lines were developed for each event. We observed short-term isotopic patterns (e.g., V-shaped trends), high-rate changes (5.3‰/h) and large absolute changes in isotopic composition (20‰) on intra-event scale. V-shaped trends appeared to be related to individual storm fronts detected by air temperature, cloud heights (NEXRAD radar echo tops) and cloud trajectories (Hybrid Single Particle Lagrangian Integrated Trajectory Model (HYSPLIT)). Despite this, we could detect no linear correlation between event-based isotopic variables (slope, δ2H-intercept, δ2H, δ18O) and the event meteoric water line. Furthermore, the composite event meteoric water line (i.e. the local meteoric water line) showed a wider spread for heavy isotopes than for light isotopes, caused presumably by different

  20. Complete assignment of NMR data of 22 phenyl-1H-pyrazoles' derivatives.

    Science.gov (United States)

    de Oliveira, Aline Lima; Alves de Oliveira, Carlos Henrique; Mairink, Laura Maia; Pazini, Francine; Menegatti, Ricardo; Lião, Luciano Morais

    2011-08-01

    Complete assignment of (1)H and (13)C NMR chemical shifts and J((1)H/(1)H and (1)H/(19)F) coupling constants for 22 1-phenyl-1H-pyrazoles' derivates were performed using the concerted application of (1)H 1D and (1)H, (13)C 2D gs-HSQC and gs-HMBC experiments. All 1-phenyl-1H-pyrazoles' derivatives were synthesized as described by Finar and co-workers. The formylated 1-phenyl-1H-pyrazoles' derivatives were performed under Duff's conditions.

  1. Temperature dependent product yields for the spin forbidden singlet channel of the C(3P) + C2H2 reaction

    Science.gov (United States)

    Hickson, Kevin M.; Loison, Jean-Christophe; Wakelam, Valentine

    2016-08-01

    The atomic hydrogen formation channels of the C + C2H2 reaction have been investigated using a continuous supersonic flow reactor over the 52-296 K temperature range. H-atoms were detected directly at 121.567 nm by vacuum ultraviolet laser induced fluorescence. Absolute H-atom yields were determined by comparison with the H-atom signal generated by the C + C2H4 reaction. The product yields agree with earlier crossed beam experiments employing universal detection methods. Incorporating these branching ratios in a gas-grain model of dense interstellar clouds increases the c-C3H abundance. This reaction is a minor source of C3-containing molecules in the present simulations.

  2. Competitive inhibition of cytosolic Ca2+-dependent phospholipase A2 by acteoside in RBL-2H3 cells.

    Science.gov (United States)

    Song, Ho Sun; Choi, Mi Young; Ko, Myoung Soo; Jeong, Jae Min; Kim, Yong Ho; Jang, Beom Hyeon; Sung, Ji Hoon; Kim, Min Gyu; Whang, Wan Kyunn; Sim, Sang Soo

    2012-05-01

    The aim of this study was to investigate whether acteoside isolated from Clerodendron trichotomum Thunberg may act as a selective inhibitor of phospholipase A(2) in RBL-2H3 cells. Acteoside dose-dependently inhibited 0.5 μM melittin-induced release of [(3)H]arachidonic acid, which was due to the inhibition of cytosolic Ca(2+)-dependent phospholipase A(2) (cPLA(2)) rather than secretory PLA(2) (sPLA(2)). In Dixon plots, the apparent K ( i ) value of acteoside on cPLA(2) was 5.9 μM and the inhibitory pattern appeared to be a competitive inhibitor. The above data, suggests that acteoside acts as a competitive inhibitor of cPLA(2) in RBL-2H3 cells.

  3. Temperature Dependent Product Yields for the Spin Forbidden Singlet Channel of the C(3P) + C2H2 Reaction

    CERN Document Server

    Hickson, Kevin M; Wakelam, Valentine

    2016-01-01

    The atomic hydrogen formation channels of the C + C2H2 reaction have been investigated using a continuous supersonic flow reactor over the 52 K 296 K temperature range. H-atoms were detected directly at 121.567 nm by vacuum ultraviolet laser induced fluorescence. Absolute H-atom yields were determined by comparison with the H-atom signal generated by the C + C2H4 reaction. The product yields agree with earlier crossed beam experiments employing universal detection methods. Incorporating these branching ratios in a gas-grain model of dense interstellar clouds increases the cC3H abundance. This reaction is a minor source of C3 containing molecules in the present simulations.

  4. Design, synthesis and evaluation of [(3)H]PF-7191, a highly specific nociceptin opioid peptide (NOP) receptor radiotracer for in vivo receptor occupancy (RO) studies.

    Science.gov (United States)

    Zhang, Lei; Drummond, Elena; Brodney, Michael A; Cianfrogna, Julie; Drozda, Susan E; Grimwood, Sarah; Vanase-Frawley, Michelle A; Villalobos, Anabella

    2014-11-15

    Herein we report the identification of (+)-N-(2-((1H-pyrazol-1-yl)methyl)-3-((1R,3r,5S)-6'-fluoro-8-azaspiro[bicyclo[3.2.1]octane-3,1'-isochroman]-8-yl)propyl)-N-[(3)H]-methylacetamide {[(3)H]PF-7191 [(+)-11]} as a promising radiotracer for the nociceptin opioid peptide (NOP) receptor. (+)-11 demonstrated high NOP binding affinity (Ki = 0.1 nM), excellent selectivity over other opioid receptors (>1000×) and good brain permeability in rats (C(b,u)/C(p,u) = 0.29). Subsequent characterization of [(3)H](+)-11 showed a high level of specific binding and a brain bio-distribution pattern consistent with known NOP receptor expression. Furthermore, the in vivo brain binding of [(3)H](+)-11 in rats was inhibited by a selective NOP receptor antagonist in a dose-responsive manner. This overall favorable profile indicated that [(3)H](+)-11 is a robust radiotracer for pre-clinical in vivo receptor occupancy (RO) measurements and a possible substrate for carbon-11 labeling for positron emission tomography (PET) imaging in higher species. Copyright © 2014 Elsevier Ltd. All rights reserved.

  5. 2-Methyl-1H-benzimidazol-3-ium hydrogen phthalate

    Directory of Open Access Journals (Sweden)

    YuanQi Yu

    2011-10-01

    Full Text Available The asymmetric unit of the title compound, C8H9N2+·C8H5O4−, contains two independent ion pairs. In each 2-methyl-1H-benzimidazolium ion, an intramolecular O—H...O bond forms an S(7 graph-set motif. In the crystal, the components are linked by N—H...O hydrogen bonds, forming chains along [210]. Further stabilization is provided by weak C—H...O hydrogen bonds.

  6. Decaying Neutralino Dark Matter in Anomalous $U(1)_H$ Models

    CERN Document Server

    Sierra, D Aristizabal; Zapata, Oscar

    2009-01-01

    In supersymmetric models extended with an anomalous $U(1)_H$ different R-parity violating couplings can yield an unstable neutralino. We show that in this context astrophysical and cosmological constraints on neutralino decaying dark matter forbid bilinear R-parity breaking neutralino decays and lead to a class of purely trilinear R-parity violating scenarios in which the neutralino is stable on cosmological scales. We have found that among the resulting models some of them become suitable to explain the observed anomalies in cosmic-ray electron/positron fluxes.

  7. Translational energy distribution from C sub 2 H sub 2 + hv(193. 3 nm) yields C sub 2 H + H

    Energy Technology Data Exchange (ETDEWEB)

    Segall, J.; Wen, Y.; Lavi, R.; Singer, R.; Wittig, C. (Univ. of Southern California, Los Angeles (United States))

    1991-10-17

    The authors report the center-of-mass translational energy distribution for 193.3-nm photolysis of expansion-cooled C{sub 2}H{sub 2}, using high-n Rydberg-level excitation of nascent H atoms to facilitate high-resolution time-of-flight measurements. The observed resolution of {approximately}200 cm{sup {minus}1} is presently limited by the ArF photolysis laser, whose band width is approximately 200 cm{sup {minus}1}. The reported distribution clearly resolves a C{sub 2}H bending progression (v{sub 2}{approximately}400 cm{sup {minus}1}), which reflects the trans-bent C{sub 2}H{sub 2} excited state. A definitive assignment of all features is still not possible on the basis of currently available information of C{sub 2}H. These measurements yield an upper bound to D{sub 0} of 131.8 {plus minus} 0.5 kcal mol{sup {minus}1}.

  8. Autoradiographic analysis of the in vivo distribution of 3H-imipramine and 3H-desipramine in brain: Comparison to in vitro binding patterns

    Energy Technology Data Exchange (ETDEWEB)

    Duncan, G.E.; Paul, I.A.; Fassberg, J.B.; Powell, K.R.; Stumpf, W.E.; Breese, G.R. (Department of Cell Biology and Anatomy, School of Medicine, University of North Carolina, Chapel Hill (USA))

    1991-03-01

    Using high resolution autoradiographic techniques, the distribution of radioactivity in forebrain and brainstem was assessed after 4 injection of 3H-impramine or 3H-desipramine. Results were compared with regional binding of the drugs to brain sections in vitro. Similar topographic binding of 3H-imipramine and 3H-desipramine was observed in vitro among brain regions, except in the paraventricular nucleus of the hypothalamus and locus coeruleus, where binding was greater for 3H-desipramine. For both 3H-desipramine and 3H-imipramine, some brain regions that exhibited high binding in vitro also showed high accumulation after in vivo injection. However, certain regions that contained high densities of binding sites for the antidepressant drugs as measured by in vitro binding showed very low accumulation of radioactivity after in vivo treatment. Such regions included the dentate gyrus of the hippocampus, layer 1 of piriform cortex, caudate-putamen, pontine and midbrain central gray, and cerebellar granular layer. Compared to in vitro binding of the drugs, the distribution of imipramine and desipramine in vivo appears more anatomically selective. For imipramine, primary sites of action in vivo, as indicated by the topographic distribution in brain, appear to be the locus coeruleus, hippocampus, lateral septal nucleus, and amygdala. For desipramine, the greatest accumulation in vivo was found in the locus coeruleus, paraventricular nucleus of the hypothalamus, and anterior thalamic nuclei.

  9. Crystal structure of rac-3-[2,3-bis(phenylsulfanyl-3H-indol-3-yl]propanoic acid

    Directory of Open Access Journals (Sweden)

    Wayland E. Noland

    2015-11-01

    Full Text Available The title compound, C23H19NO2S2, was obtained as an unexpected regioisomer from an attempted synthesis of an intermediate for a substituent-effect study on ergot alkaloids. This is the first report of a 1H-indole monothioating at the 2- and 3-positions to give a 3H-indole. In the crystal, the acid H atom is twisted roughly 180° from the typical carboxy conformation and forms centrosymmetric O—H...N hydrogen-bonded dimers with the indole N atom of an inversion-related molecule. Together with a weak C—H...O hydrogen bond involving the carbonyl O atom, chains are formed along [100].

  10. SMA OBSERVATIONS OF THE W3(OH) COMPLEX: PHYSICAL AND CHEMICAL DIFFERENTIATION BETWEEN W3(H{sub 2}O) AND W3(OH)

    Energy Technology Data Exchange (ETDEWEB)

    Qin, Sheng-Li [Department of Astronomy, Yunnan University, and Key Laboratory of Astroparticle Physics of Yunnan Province, Kunming, 650091 (China); Schilke, Peter; Sánchez-Monge, Álvaro [Physikalisches Institut, Universität zu Köln, Zülpicher Str. 77, D-50937 Köln (Germany); Wu, Jingwen [Department of Physics and Astronomy, University of California, Los Angeles, CA 90095 (United States); Wu, Yuefang [Department of Astronomy, Peking University, Beijing, 100871 (China); Liu, Tie [Korea Astronomy and Space Science Institute 776, Daedeokdaero, Yuseong-gu, Daejeon, Korea 305-348 (Korea, Republic of); Liu, Ying, E-mail: slqin@bao.ac.cn [Department of Physics and Hebei Advanced Thin Film Laboratory, Hebei Normal University, Shijiazhuang 050024 (China)

    2015-04-10

    We report on the Submillimeter Array (SMA) observations of molecular lines at 270 GHz toward the W3(OH) and W3(H{sub 2}O) complex. Although previous observations already resolved the W3(H{sub 2}O) into two or three sub-components, the physical and chemical properties of the two sources are not well constrained. Our SMA observations clearly resolved the W3(OH) and W3(H{sub 2}O) continuum cores. Taking advantage of the line fitting tool XCLASS, we identified and modeled a rich molecular spectrum in this complex, including multiple CH{sub 3}CN and CH{sub 3}OH transitions in both cores. HDO, C{sub 2}H{sub 5}CN, O{sup 13}CS, and vibrationally excited lines of HCN, CH{sub 3}CN, and CH{sub 3}OCHO were only detected in W3(H{sub 2}O). We calculate gas temperatures and column densities for both cores. The results show that W3(H{sub 2}O) has higher gas temperatures and larger column densities than W3(OH) as previously observed, suggesting physical and chemical differences between the two cores. We compare the molecular abundances in W3(H{sub 2}O) to those in the Sgr B2(N) hot core, the Orion KL hot core, and the Orion Compact Ridge, and discuss the chemical origin of specific species. An east–west velocity gradient is seen in W3(H{sub 2}O), and the extension is consistent with the bipolar outflow orientation traced by water masers and radio jets. A north–south velocity gradient across W3(OH) is also observed. However, with current observations we cannot be assured whether the velocity gradients are caused by rotation, outflow, or radial velocity differences of the sub-components of W3(OH)

  11. Profiling formulated monoclonal antibodies by (1)H NMR spectroscopy.

    Science.gov (United States)

    Poppe, Leszek; Jordan, John B; Lawson, Ken; Jerums, Matthew; Apostol, Izydor; Schnier, Paul D

    2013-10-15

    Nuclear magnetic resonance (NMR) is arguably the most direct methodology for characterizing the higher-order structure of proteins in solution. Structural characterization of proteins by NMR typically utilizes heteronuclear experiments. However, for formulated monoclonal antibody (mAb) therapeutics, the use of these approaches is not currently tenable due to the requirements of isotope labeling, the large size of the proteins, and the restraints imposed by various formulations. Here, we present a new strategy to characterize formulated mAbs using (1)H NMR. This method, based on the pulsed field gradient stimulated echo (PGSTE) experiment, facilitates the use of (1)H NMR to generate highly resolved spectra of intact mAbs in their formulation buffers. This method of data acquisition, along with postacquisition signal processing, allows the generation of structural and hydrodynamic profiles of antibodies. We demonstrate how variation of the PGSTE pulse sequence parameters allows proton relaxation rates and relative diffusion coefficients to be obtained in a simple fashion. This new methodology can be used as a robust way to compare and characterize mAb therapeutics.

  12. 23Na and 1H NMR Microimaging of Intact Plants

    Science.gov (United States)

    Olt, Silvia; Krötz, Eva; Komor, Ewald; Rokitta, Markus; Haase, Axel

    2000-06-01

    23Na NMR microimaging is described to map, for the first time, the sodium distribution in living plants. As an example, the response of 6-day-old seedlings of Ricinus communis to exposure to sodium chloride concentrations from 5 to 300 mM was observed in vivo using 23Na as well as 1H NMR microimaging. Experiments were performed at 11.75 T with a double resonant 23Na-1H probehead. The probehead was homebuilt and equipped with a climate chamber. T1 and T2 of 23Na were measured in the cross section of the hypocotyl. Within 85 min 23Na images with an in-plane resolution of 156 × 156 μm were acquired. With this spatial information, the different types of tissue in the hypocotyl can be discerned. The measurement time appears to be short compared to the time scale of sodium uptake and accumulation in the plant so that the kinetics of salt stress can be followed. In conclusion, 23Na NMR microimaging promises great potential for physiological studies of the consequences of salt stress on the macroscopic level and thus may become a unique tool for characterizing plants with respect to salt tolerance and salt sensitivity.

  13. Metabolomic insight into soy sauce through (1)H NMR spectroscopy.

    Science.gov (United States)

    Ko, Bong-Kuk; Ahn, Hyuk-Jin; van den Berg, Frans; Lee, Cherl-Ho; Hong, Young-Shick

    2009-08-12

    Soy sauce, a well-known seasoning in Asia and throughout the world, consists of many metabolites that are produced during fermentation or aging and that have various health benefits. However, their comprehensive assessment has been limited due to targeted or instrumentally specific analysis. This paper presents for the first time a metabolic characterization of soy sauce, especially that aged up to 12 years, to obtain a global understanding of the metabolic variations through (1)H NMR spectroscopy coupled with multivariate pattern recognition techniques. Elevated amino acids and organic acids and the consumption of carbohydrate were associated with continuous involvement of microflora in aging for 12 years. In particular, continuous increases in the levels of betaine were found during aging for up to 12 years, demonstrating that microbial- or enzyme-related metabolites were also coupled with osmotolerant or halophilic bacteria present during aging. This work provides global insights into soy sauce through a (1)H NMR-based metabolomic approach that enhances the current understanding of the holistic metabolome and allows assessment of soy sauce quality.

  14. The H{sup +}{sub 3} + H{sub 2} isotopic system. Origin of deuterium astrochemistry

    Energy Technology Data Exchange (ETDEWEB)

    Hugo, Edouard Jean-Marie

    2008-07-01

    Dense cold molecular clouds reckoned to be stellar nurseries are the scene of an extreme molecular deuteration. Despite the cosmic D/H ratio of {proportional_to}10{sup -5}, molecular species in prestellar cores are observed to contain nearly as much deuterium as hydrogen. This astonishing deuterium enrichment promoted by low temperatures is the work of H{sup +}{sub 3}. It is the key species which unlocks the deuterium from its HD reservoir via reactions like H{sup +}{sub 3}+HD {r_reversible} H{sub 2}D{sup +}+H{sub 2} and drags it further to other species in successive reactions. For this reason, the H{sup +}{sub 3}+H{sub 2} isotopic system is outstandingly critical for the astrochemistry of cold environments. However, its understanding is yet incomplete and insufficient. This thesis thus focuses on the H{sup +}{sub 3}+H{sub 2} isotopic system from a theoretical, experimental and astronomical point of view giving a particular look into the role of nuclear spins. As a first step, the stringent nuclear spin selection rules in associative, dissociative and reactive collisions are investigated. This purely theoretical study zooms into the details of the nuclear spin wavefunctions and shows that their permutation symmetry representation is necessary and sufficient, contrary to their angular momentum representation. Additionally, a new deterministic interpretation of nuclear spins in chemical reactions is proposed. Based on these considerations, a complete set of state-to-state rate coefficients for all H{sup +}{sub 3} + H{sub 2} isotopic variants is calculated using a microcanonical model leaned on phase space theory. An experimental study is conducted in parallel with a 22-pole ion trap apparatus in order to inspect the influences of temperature and H{sub 2} ortho-to-para ratio. The good overall agreement between experimental and theoretical results supports the validity and utility of the calculated set of rate coefficients. Furthermore, the potentiality of the 22-pole

  15. CN and C2H in IRC +10216

    Science.gov (United States)

    Huggins, P. J.; Glassgold, A. E.; Morris, M.

    1984-01-01

    The effects of the production of the radicals CN and C2H from the dissociation of HCN and C2H2 by ambient UV photons in the outer envelope of IRC +10216 are investigated. The spatial distribution of the radicals and their observable millimeter emission-line characteristics are calculated from the inferred abundances of the progenitor species in the envelope of IRC +10216 using photochemical and radiative transfer models. These are compared with available observations to examine whether photoproduction is a possible explanation of the observed emission from these species. The results suggest that the variable abundances induced by photodestruction of their progenitors do affect the observed emission from the radicals.

  16. Reatividade de 2H-azirinas-funcionalizadas com hidrazinas

    OpenAIRE

    Cecilia Maria Alves de Oliveira

    1987-01-01

    Resumo: As azirinas são intermediários sintéticos importantes na química de heterocíclicos. No presente trabalho, reações de 3-fenil-2-formil-2H-azirina(41) e 3-fenil-2-formil-2-metil-2H-azirina(42) que possuem um grupo aldeído na posição 2 do anel, são investigadas. A reação de (41) com hidrazina leva a 4-amino-3-fenil-pirazol (57) e a reação de (42), que possui um substituinte metila adicional na posição 2 do anel, com o mesmo nucleófilo leva a 1,4-dihidro 3-fenil-5-metil-1,2,4-triazina (72...

  17. Charge transfer in energetic Li^2+ - H collisions

    Science.gov (United States)

    Mancev, I.

    2008-07-01

    The total cross sections for charge transfer in Li^2+ - H collisions have been calculated, using the four-body first Born approximation with correct boundary conditions (CB1-4B) and four-body continuum distorted wave method (CDW-4B) in the energy range 10 - 5000 keV/amu. Present results call for additional experimental data at higher impact energies than presently available.

  18. Electron-Deficient Iron Alkyl Complexes Supported by Diimine Ligand (Ph2CN)(2)C2H4 : Evidence for Reversible Ethylene Binding

    NARCIS (Netherlands)

    Volbeda, Jeroen; Meetsma, Auke; Bouwkamp, Marco W.

    2009-01-01

    Reaction of diimine ligands (Ph2CN)(2)CnH2n (n = 2, a; n = 3, b) with FeCl2 or FeBr2 results in formation of the corresponding high-spin ferrous complexes {Ph2CN)(2)C2H4} FeX2 (1a, X = Cl; 2a, X = Br) and {(Ph2CN)(2)C3H3}FeCl2 (1b). Dialkyl {(Ph2CN)(2)C2H4) Fe(CH2SiMe3)(2) (3a) was prepared by

  19. A Metalloradical Approach to 2H-Chromenes

    Science.gov (United States)

    Paul, Nanda D.; Mandal, Sutanuva; Otte, Matthias; Cui, Xin; Zhang, X. Peter; de Bruin, Bas

    2014-01-01

    Cobalt(III)–carbene radicals, generated through metalloradical activation of salicyl N-tosylhydrazones by cobalt(II) complexes of porphyrins, readily undergo radical addition to terminal alkynes to produce salicyl-vinyl radical intermediates. Subsequent hydrogen atom transfer (HAT) from the hydroxy group of the salicyl-moiety to the vinyl-radical leads to the formation of 2H-chromenes. The Co(II)-catalyzed process can tolerate various substitution patterns and produces the corresponding 2H-chromene products in good isolated yields. EPR spectroscopy and radical-trapping experiments with TEMPO are in agreement with the proposed radical mechanism. DFT calculations reveal the formation of the salicyl-vinyl radical intermediate by a metalloradical mediated process. Unexpectedly, subsequent HAT from the hydroxy moiety to the vinyl radical leads to formation of an o-quinone methide intermediate, which dissociates spontaneously from the cobalt center and easily undergoes an endo-cyclic, sigmatropic ring-closing reaction to form the final 2H-chromene product. PMID:24400781

  20. Microwave-assisted synthesis of novel 5-trichloromethyl-4,5-dihydro-1H-1-pyrazole methyl esters under solvent free conditions

    Energy Technology Data Exchange (ETDEWEB)

    Martins, Marcos A.P.; Beck, Paulo; Machado, Pablo; Brondani, Sergio; Moura, Sidnei; Zanatta, Nilo; Bonacorso, Helio G.; Flores, Alex F.C. [Universidade Federal de Santa Maria, RS (Brazil). Dept. de Quimica. Nicleo de Quimica de Heterociclos (NUQUIMHE)]. E-mail: mmartins@base.ufsm.br

    2006-03-15

    Twelve novel 5-trichloromethyl-4,5-dihydro-1H-1-pyrazole ethyl esters have been synthesized in good yields (70-98%) by using environmentally benign microwave induced techniques. The compounds were synthesized from the cyclocondensation of 1,1,1-trichloro-4-alkoxy-3-alken-2-ones [CCl3{sub C}(O)C(R{sup 2})=C(R{sup 1} )OR, where R, R{sup 2} = H, alkyl; R{sup 1} = H, alkyl and aryl] with hydrazine methyl carboxylate. The advantages obtained by the using of microwave irradiation under solvent-free conditions, rather than a conventional method, were demonstrated. (author)

  1. Genetic Variation in Myosin 1H Contributes to Mandibular Prognathism

    Science.gov (United States)

    Tassopoulou-Fishell, Maria; Deeley, Kathleen; Harvey, Erika M.; Sciote, James; Vieira, Alexandre R.

    2013-01-01

    Introduction Several candidate loci have been suggested as influencing mandibular prognathism (1p22.1, 1p22.2, 1p36, 3q26.2, 5p13-p12, 6q25, 11q22.2-q22.3, 12q23, 12q13.13, and 19p13.2). The goal of this study was to replicate these results in a well-characterized homogeneous sample set. Methods Thirty-three single nucleotide polymorphisms spanning all candidate regions were studied in 44 prognathic and 35 Class I subjects from the University of Pittsburgh School of Dental Medicine Dental Registry and DNA Repository. The 44 mandibular prognathism subjects had an average age of 18.4 years, 31 were females and 13 males, and 24 were White, 15 African American, two Hispanic, and three Asian. The 35 Class I subjects had an average age of 17.6 years, 27 were females and 9 males, and 27 were White, six African Americans, one Hispanic, and two Asian. Skeletal mandibular prognathism diagnosis included cephalometric values indicative of Class III such as ANB smaller than two degrees, negative Witts appraisal, and positive A–B plane. Additional mandibular prognathism criteria included negative OJ and visually prognathic (concave) profile as determined by the subject's clinical evaluation. Orthognathic subjects without jaw deformations were used as a comparison group. Mandibular prognathism and orthognathic subjects were matched based on race, sex and age. Genetic markers were tested by polymerase chain reaction using TaqMan chemistry. Chi-square and Fisher exact tests were used to determine overrepresentation of marker allele with alpha of 0.05. Results An association was unveiled between a marker in MYO1H (rs10850110) and the mandibular prognathism phenotype (p=0.03). MYO1H is a Class-I myosin that is in a different protein group than the myosin isoforms of muscle sarcomeres, which are the basis of skeletal muscle fiber typing. Class I myosins are necessary for cell motility, phagocytosis and vesicle transport. Conclusions More strict clinical definitions may increase

  2. Comparison of high affinity binding of {sup 3}H-proadifen and {sup 3}H-(-)-cocaine t rat liver membranes

    Energy Technology Data Exchange (ETDEWEB)

    Ross, S.B. [Astra Arcus AB, Dept. of Neuropharmacology, Soedertaelje (Sweden)

    1995-06-01

    The characteristics of the binding of {sup 3}H-proadifen to rat liver membranes were studied and compared to those of {sup 3}H-cocaine. It was found that {sup 3}H-proadifen was bound reversibly with high affinity (K{sub D}=1.8{+-}0.5 nM) and large capacity (B{sub max}=2010{+-}340 pmol/g wet tissue) to liver membranes. The corresponding values for the {sup 3}H-cocaine binding were 3.5 nM and 1000 pmol/g wet tissue. The binding of {sup 3}H-proadifen was mainly localised to the microsomal fraction. The number of binding sites was not increased by treatment of rats with phenobarbitone. With 1 {mu}M CdCl{sub 2} in the incubation buffer it was possible to differentiate between two {sup 3}H-cocaine binding sites with K{sub d} values of 1.6 and 7.7 nM and B{sub max} values of 280 and 940 pmol/g wet liver tissue. S-(-)-Alaproclate inhibited the binding of {sup 3}H-proadifen and {sup 3}H-cocaine inhibited the binding of {sup 3}H-proadifen (IC{sub 50}=10 nM) and proadifen that of {sup 3}H-cocaine (IC{sub 50}=1 nM). There was a high correlation coefficient (r{sub r}=0.972; P<0.01; n=12) in the Spearman rank test between the inhibitory potencies of compounds examined in both systems. Beside some potent alaproclate analogues a couple of compounds had moderately high affinity (IC{sub 50}=100-500 nM): chloroquine, phenoxybenzamine, amitriptyline, ajmaline, remoxipride, imipramine and (-)-alaprenolol. CdCl{sub 2}, ZnCl{sub 2} and CuCl{sub 2} inhibited the binding of both ligands with low Hill coefficients, indicating heterogeneous binding sites. The inhibition curve of Cd{sup 2+} on the cocaine binding was biphasic with a high affinity part around 50 nM and a low affinity part at 15{mu}M. The similarity of the characteristics of the binding of these ligands with that of {sup 3}H-alaproclate is discussed. It is suggested that all three compounds bind to the same sites, although additional binding sites seem to exist for proadifen. (au) (9 refs.).

  3. Crystal structure of 1H,1'H-[2,2'-biimid-azol]-3-ium hydrogen tartrate hemi-hydrate.

    Science.gov (United States)

    Gao, Xiao-Li; Bian, Li-Fang; Guo, Shao-Wei

    2014-11-01

    In the crystal of the title hydrated salt, C6H7N4 (+)·C4H5O6 (-)·0.5H2O, the bi-imidazole monocation, 1H,1'H-[2,2'-biimidazol]-3-ium, is hydrogen bonded, via N-H⋯O, O-H⋯O and O-H⋯N hydrogen bonds, to the hydrogen tartrate anion and the water mol-ecule, which is located on a twofold rotation axis, forming sheets parallel to (001). The sheets are linked via C-H⋯O hydrogen bonds, forming a three-dimensional structure. There are also C=O⋯π inter-actions present [O⋯π distances are 3.00 (9) and 3.21 (7) Å], involving the carbonyl O atoms and the imidazolium ring, which may help to consolidate the structure. In the cation, the dihedral angle between the rings is 11.6 (2)°.

  4. Synthesis and antifungal activity of 2H-1,4-benzoxazin-3(4H)-one derivatives.

    Science.gov (United States)

    Śmist, Małgorzata; Kwiecień, Halina; Krawczyk, Maria

    2016-01-01

    A series of 2-alkyl-2H-1,4-benzoxazin-3(4H)-ones (4a-l) was easily synthesized by two-step process involving O-alkylation of 2-nitrophenols with methyl 2-bromoalkanoates and next "green" catalytic reductive cyclization of the obtained 2-nitro ester intermediates (3a-l). Further, 6,7-dibromo (5a-c) and N-acetyl (6) derivatives were prepared by bromination and acetylation of unsubstituted 2-alkyl-2H-1,4-benzoxazin-3(4H)-ones (4a-c). The novel compounds (3a-l, 4d-l, 5a-c and 6) were fully characterized by spectroscopic methods (MS, (1)H and (13)C NMR). 2-Alkyl-2H-1,4-benzoxazin-3(4H)-ones (4a-l, 5a-c and 6) were screened for antifungal activity. Preliminary assays were performed using two methods: in vitro against seven phytopathogenic fungi-Botrytis cinerea, Phythophtora cactorum, Rhizoctonia solani, Phoma betae, Fusarium culmorum, Fusarium oxysporum and Alternaria alternata-and in vivo against barley powdery mildew Blumeria graminis. The tested compounds displayed moderate to good antifungal activity at high concentration (200 mg L(-1)). The most potent compounds were 2-ethyl-2H-1,4-benzoxazin-3(4H)-one (4a), 2-ethyl-7-fluoro-2H-1,4-benzoxazin-3(4H)-one (4g) and 4-acetyl-2-ethyl-2H-1,4-benzoxazin-3(4H)-one (6), which completely inhibited the mycelial growth of seven agricultural fungi at the concentration of 200 mg L(-1) in the in vitro tests. Moreover, 2-ethyl-2H-1,4-benzoxazin-3(4H)-one (4a) and 4-acetyl-2-ethyl-2H-1,4-benzoxazin-3(4H)-one (6) were also screened for antifungal activity at concentrations of 100 mg L(-1) and 20 mg L(-1). In the concentration of 100 mg L(-1), the N-acetyl derivative (6) completely inhibited the growth of three strains of fungi (F. culmorum, P. cactorum and R. solani), while 2-ethyl-2H-1,4-benzoxazin-3(4H)-one (4a) completely inhibited only R. solani strain. At the concentration of 20 mg L(-1), compound 6 showed good activity only against P. cactorum strain (72%).

  5. In2S3-H2O系电位-pH图%Potential-pH diagrams of In2S3-H2O system

    Institute of Scientific and Technical Information of China (English)

    俞小花; 谢刚; 李永刚; 杨大锦; 刘春侠

    2008-01-01

    通过热力学计算,给出了In2S3-H2O系的反应平衡式及电位-pH的关系式,并绘制了25 ℃和150 ℃下In2S3-H2O系的电位-pH图,为含硫化铟的矿物高温氧化浸出提供了一定的热力学数据.

  6. 4-Methyl-5-phenyl-1H-pyrazol-3-ol

    Directory of Open Access Journals (Sweden)

    Tara Shahani

    2010-07-01

    Full Text Available The title compound, C10H10N2O, crystallizes with two independent molecules in the asymmetric unit, having closely comparable geometries. The dihedral angles between the 1H-pyrazole and benzene rings in the two molecules are 39.57 (14 and 41.95 (13°. The two molecules are each connected to neighbouring molecules by pairs of intermolecular O—H...N hydrogen bonds, forming dimers with R22(8 ring motifs. These dimers are further linked into R44(10 ring motifs by intermolecular N—H...O hydrogen bonds, forming chains along [101]. The crystal structure is further stabilized by a C—H...π interaction.

  7. Experimental cross-sections energy dependence and an ab initio electronic structure survey of the ground singlet potential surface for reactive Li(+) + n-C(3)H(7)Cl collisions at low energies.

    Science.gov (United States)

    Lucas, José María; de Andrés, Jaime; Albertí, Margarita; Bofill, Josep Maria; Bassi, Davide; Aguilar, Antonio

    2010-11-07

    Reactive collisions between n-C(3)H(7)Cl molecules and lithium ions both in their ground electronic state have been studied in the 0.05-7.00 eV center of mass energy range using an octopole radio frequency guided-ion beam apparatus developed in our laboratory and recently modified. At low collision energies, dehydrohalogenation reactions leading to Li(C(3)H(6))(+) and Li(HCl)(+) are the main reaction channels, while on increasing energies C(3)H(7)(+) and C(2)H(3)(+) formation become dominant. Cross section energy dependences in arbitrary units for all these reactions have been measured. Also, ab initio electronic structure calculations at the MP2 level have been performed to obtain information about the potential energy surface on which the reactive processes take place. The reactants' entrance channel leads to the formation of a stable [Li-n-C(3)H(7)Cl](+) ion-molecule adduct that, following an intrinsic-reaction-coordinate pathway and surmounting a transition state, isomerizes to [Li-i-C(3)H(7)Cl](+). From this second minimum, dehydrohalogenation reactions for both n-C(3)H(7)Cl and i-C(3)H(7)Cl share a common reaction pathway leading to the same products. All potential barriers explored by reactions always lie below the reactants' energy. The entrance reaction channel [Li-n-C(3)H(7)Cl](+) adduct also leads adiabatically to C(3)H(7)(+) formation which, on increasing collision energy generates C(2)H(3)(+)via a unimolecular decomposition. A qualitative interpretation of the experimental results based on our ab initio calculations is also given.

  8. Syntheses, structures, and properties of six cobalt(II) complexes based on a tripodal tris(4-(1H-1,2,4-triazol-1-yl)phenyl)amine ligand.

    Science.gov (United States)

    Shi, Zhenzhen; Pan, Zhaorui; Zhang, Chuanlei; Zheng, Hegen

    2015-10-14

    Six new cobalt(ii) metal-organic frameworks, {[Co1.5(TTPA)(BTC)(H2O)]2·13H2O}n (1), [Co(TTPA)(PA)]n (2), {[Co(TTPA)(BDA)0.5(NO3)]·3H2O}n (3), {[Co2(TTPA)3(OBA)2(H2O)3]·2CH3CN·4H2O}n (4), {[Co(TTPA)(AIP)(H2O)]·2H2O}n (5), and {[Co(TTPA)(MIP)(H2O)]·2H2O}n (6), have been prepared by the self-assembly of a tris(4-(1H-1,2,4-triazol-1-yl)phenyl)amine (TTPA) ligand with different aromatic carboxylate auxiliary ligands (H3BTC = 1,3,5-benzenetricarboxylic acid, H2PA = phthalic acid, H2BDA = (1,1'-biphenyl)-4,4'-dicarboxylic acid, H2OBA = 4,4'-oxydibenzoic acid, H2AIP = 5-aminoisophthalic acid, H2MIP = 5-methylisophthalic acid) and cobalt salts. Their structures have been characterized by infrared spectroscopy, elemental analysis, single crystal X-ray analysis, and powder X-ray diffraction. Complex 1 is an unusual 4-nodal (3,3,4,8)-connected three-dimensional (3D) new topological net with the point symbol of (4·6·8)4(4(4)·6(7)·8(15)·10(2))(6(2)·8(4)). Complex 2 has a 2-fold interpenetrating 3D dia framework. Complex 3 displays a rare binodal (3,4)-connected 4-fold interpenetrating 3D architecture with a fsc-3,4-C2/c topology with the point symbol of (4·6·8)(4·6(2)·8(3)). Complex 4 shows two distinct two-dimensional (2D) layers with hcb topologies, which are further packed into a 3D structure by O-HO hydrogen bonding interactions. Both complexes 5 and 6 feature similar 2D sheets with sql topologies, which can be further packed into a 3D structure by O-HO hydrogen bonding interactions. Moreover, the thermal stability and UV-visible spectra of these complexes are also discussed in detail. Meanwhile, the variable-temperature magnetic susceptibility measurement of complex 1 reveals antiferromagnetic interactions between Co(ii) ions.

  9. Characterization of (/sup 3/H)pirenzepine binding to muscarinic cholinergic receptors solubilized from rat brain

    Energy Technology Data Exchange (ETDEWEB)

    Luthin, G.R.; Wolfe, B.B.

    1985-07-01

    Membranes prepared from rat cerebral cortex were solubilized in buffer containing 1% digitonin. Material present in the supernatant after centrifugation at 147,000 X g was shown to contain binding sites for both (/sup 3/H)quinuclidinyl benzilate ((/sup 3/H)QNB) and (/sup 3/H)pirenzepine ((/sup 3/H)PZ). Recovery of binding sites was approximately 25% of the initial membrane-bound (/sup 3/H)QNB binding sites. The Kd values for (/sup 3/H)QNB and (/sup 3/H)PZ binding to solubilized receptors were 0.3 nM and 0.1 microM, respectively. As has been observed previously in membrane preparations, (/sup 3/H)PZ appeared to label fewer solubilized binding sites than did (/sup 3/H)QNB. Maximum binding values for (/sup 3/H)PZ and (/sup 3/H)QNB binding to solubilized receptors were approximately 400 and 950 fmol/mg of protein, respectively. Competition curves for PZ inhibiting the binding of (/sup 3/H)QNB, however, had Hill slopes of 1, with a Ki value of 0.24 microM. The k1 and k-1 for (/sup 3/H)PZ binding were 3.5 X 10(6) M-1 min-1 and 0.13 min-1, respectively. The muscarinic receptor antagonists atropine, scopolamine and PZ inhibited the binding of (/sup 3/H)QNB and (/sup 3/H)PZ to solubilized receptors with Hill slopes of 1, as did the muscarinic receptor agonist oxotremorine. The muscarinic receptor agonist carbachol competed for (/sup 3/H)QNB and (/sup 3/H)PZ binding with a Hill slope of less than 1 in cerebral cortex, but not in cerebellum. GTP did not alter the interactions of carbachol or oxotremorine with the solubilized receptor. Together, these data suggest that muscarinic receptor sites solubilized from rat brain retain their abilities to interact selectively with muscarinic receptor agonists and antagonists.

  10. Hydrogenation and Deuteration of C2H2 and C2H4 on Cold Grains: A Clue to the Formation Mechanism of C2H6 with Astronomical Interest

    Science.gov (United States)

    Kobayashi, Hitomi; Hidaka, Hiroshi; Lamberts, Thanja; Hama, Tetsuya; Kawakita, Hideyo; Kästner, Johannes; Watanabe, Naoki

    2017-03-01

    We quantitatively investigated the hydrogen addition reactions of acetylene (C2H2) and ethylene (C2H4) on amorphous solid water (ASW) at 10 and 20 K relevant to the formation of ethane (C2H6) on interstellar icy grains. We found that the ASW surface enhances the reaction rates for C2H2 and C2H4 by approximately a factor of 2 compared to those on the pure-solid C2H2 and C2H4 at 10 K, probably due to an increase in the sticking coefficient and adsorption energy of the H atoms on ASW. In contrast to the previous proposal that the hydrogenation rate of C2H4 is orders of magnitude larger than that of C2H2, the present results show that the difference in hydrogenation rates of C2H2 and C2H4 is only within a factor of 3 on both the surfaces of pure solids and ASW. In addition, we found the small kinetic isotope effect for hydrogenation/deuteration of C2H2 and C2H4 at 10 K, despite the requirement of quantum tunneling. At 20 K, the reaction rate of deuteration becomes even larger than that of hydrogenation. These unusual isotope effects might originate from a slightly larger number density of D atoms than H atoms on ASW at 20 K. The hydrogenation of C2H2 is four times faster than CO hydrogenation and can produce C2H6 efficiently through C2H4 even in the environment of a dark molecular cloud.

  11. Misoprostol 1 to 3 h preprocedure vs. overnight osmotic dilators prior to early second-trimester surgical abortion.

    Science.gov (United States)

    Ramesh, Shanthi; Roston, Alicia; Zimmerman, Lindsay; Patel, Ashlesha; Lichtenberg, E Steve; Chor, Julie

    2015-09-01

    We sought to compare the effectiveness of at least 1 h of 400 mcg of buccal misoprostol to overnight osmotic dilators for early second-trimester surgical abortion cervical preparation. We conducted a retrospective cohort study, reviewing 145 consecutive charts to compare procedure duration for women who received 400 mcg of buccal misoprostol at least 1 h preprocedure vs. overnight osmotic dilators before dilation and evacuation between 14 weeks, 0 days and 15 weeks, 6 days' gestation. Primary outcome was procedure duration and secondary outcomes included maximum mechanical dilator size, estimated blood loss and side effects. Sixty-four women (44.1%) received buccal misoprostol (mean 1.6 h), and 81 women (55.9%) received overnight osmotic dilators. Groups did not differ regarding mean gestational age or gynecologic history. All procedures in both groups were completed. Procedure duration was not significantly different between the misoprostol and osmotic dilator groups (median 11.0 min vs. 10.0 min, p=.22), even after multivariable linear regression (p=.17). The mean total cervical preparation duration was 1.6 h for women in the misoprostol group compared to 20.3 h in the osmotic dilator group (pmisoprostol decreased the duration of cervical preparation for early second-trimester procedures performed by an experienced surgeon. In this small, retrospective review, at least 1 h of preprocedure buccal misoprostol decreased the duration from cervical preparation initiation to procedure completion in early second-trimester procedures performed by an experienced surgeon. These results should be considered as a pilot evaluation, and further prospective study is needed to further clarify whether this short interval could be applied in general practice. Copyright © 2015 Elsevier Inc. All rights reserved.

  12. Menthyl 2-oxo-2H-chromene-3-carboxylate

    Directory of Open Access Journals (Sweden)

    Cui-Lian Xu

    2009-10-01

    Full Text Available The title compound, C20H24O4, was synthesized from the reaction of 2-oxo-2H-chromene-3-acyl chloride and menthol. The mean plane of the ester group and that of the four essentially planar (maximum deviation 0.0112 Å C atoms of the chair-form cyclohexyl ring form dihedral angles of 43.8 (3 ° and 81.8 (1°, respectively, with the mean plane of the coumarin ring system. In the crystal structure, weak intermolecular C—H...O hydrogen bonds connect the molecules into a two-dimensional network.

  13. Multiobjective H2/H? Control Design with Regional Pole Constraints

    Directory of Open Access Journals (Sweden)

    Junaidi Junaidi

    2012-03-01

    Full Text Available This paper presents multiobjective H2/H? control design with regional pole constraints. The state feedback gain can be obtained by solving a linear matrix inequality (LMI feasibility problem that robustly assigns the closed-loop poles in a prescribed LMI region. The proposed technique is illustrated with applications to the design of stabilizer for a typical single-machine infinite-bus (SMIB power system. The LMI-based control ensures adequate damping for widely varying system operating conditions. The simulation results illustrate the effectiveness and robustness of the proposed stabilizer.

  14. Thermodynamic properties and crystal structure refinement of ferricopiapite, coquimbite, rhomboclase, and Fe2(SO4)3(H2O)5

    Science.gov (United States)

    Majzlan, J.; Navrotsky, A.; McCleskey, R.B.; Alpers, C.N.

    2006-01-01

    Enthalpies of formation of ferricopiapite [nominally Fe4.67(SO4)6(OH)2 (H2O)20]. coquimbite [Fe2(SO4)3(H2O)9], rhomboclase [(H3O)Fe(SO4)2 (H2O)3], and Fe2(SO4)3(H2O)5 were measured by acid (5 N HCl) solution calorimetry. The samples were characterized by wet chemical analyses and synchrotron powder X-ray diffraction (XRD). The refinement of XRD patterns gave lattice parameters, atomic positions, thermal factors, and occupancies of the sites. The calculated formulae differ slightly from the nominal compositions: Fe4.78(SO4)6 (OH)2.34(H2O)20.71 (ferricopiapite), (Fe1.47Al0.53)(SO4)3 (H2O)9.65 (coquimbite), (H3O)1.34Fe(SO4)2.17 (H2O)3.06 (rhomboclase), and Fe2(SO4)3 (H2O)5.03. All thermodynamic data are given per mole of these formulae. The measured standard enthalpies (in kJ/mol) of formation from the elements (crystalline Fe, Al, S, and ideal gases O2 and H2) at T = 298.15 K are -4115.8??4.1 [Fe2(SO4)3 (H2O)5.03], -12045.1??9.2 (ferricopiapite), -5738.4??3.3 (coquimbite), and -3201.1??2.6 (rhomboclase). Standard entropy (S??) was estimated as a sum of entropies of oxide, hydroxide, and sulfate components. The estimated S?? (in J/mol.K) values for the iron sulfates are 488.2 [Fe2(SO4)3 (H2O)5.03], 1449.2 (ferricopiapite), 638.3 (coquimbite), and 380.1 (rhomboclase). The calculated Gibbs free energies of formation (in kJ/mol) are -3499.7??4.2 [Fe2(SO4)3 (H2O)5.03], -10089.8??9.3 (ferricopiapite), -4845.6??3.3 (coquimbite), and -2688.0??2.7 (rhomboclase). These results combined with other available thermodynamic data allow construction of mineral stability diagrams in the FeIII2(SO4)3-FeII SO4-H2O system. One such diagram is provided, indicating that the order of stability of ferric sulfate minerals with decreasing pH in the range of 1.5 to -0.5 is: hydronium jarosite, ferricopiapite, and rhomboclase. ?? 2006 E. Schweizerbart'sche Verlagsbuchhandlung.

  15. Synthesis and Characterization of a Novel Copoly(aryl ether ketone) Containing 4, 4'-Biphenyl-bis[4-phthalazin-1(2H)-one] Moiety

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    A new monomer of 4, 4'-biphenyl-bis[4-phthalazin-1(2H)-one] was synthesized from biphenyl and phthalic anhydride, and a novel copoly(aryl ether ketone) (PPEK) was synthesized from 2, 2-bis(4-hydroxyphenyl)-propane (BPA), 4, 4'-biphenyl-bis-[4-phthalazin-1(2H)-one], 4, 4'- difluorodiphenylketone (DFK). The monomer and copolymer were characterized by FT-IR and 1H-NMR. DSC and TGA were used to the novel polymer.

  16. catena-Poly[[[diaqua-copper(II)]-bis-[μ-1,5-bis-(1H-imidazol-1-yl)pentane-κ(2) N (3):N (3')

    National Research Council Canada - National Science Library

    Zhang, Lai-Ping; Wen, Shu-Tang; Fu, Xiao-Ning

    2012-01-01

    In the title complex, {[Cu(C11H16N4)2(H2O)2](C10H6O6S2)} n , the Cu(II) atom, lying on an inversion center, is six-coordinated by two water mol-ecules and four N atoms from four 1,5-bis-(1H-imidazol-1-yl)pentane (biim-5...

  17. A new one-dimensional Cd(II) coordination polymer with a two-dimensional layered structure incorporating 2-[(1H-imidazol-1-yl)methyl]-1H-benzimidazole and benzene-1,2-dicarboxylate ligands.

    Science.gov (United States)

    Huang, Qiu Ying; Lin, Xiao Yi; Meng, Xiang Ru

    2016-06-01

    The N-heterocyclic ligand 2-[(1H-imidazol-1-yl)methyl]-1H-benzimidazole (imb) has a rich variety of coordination modes and can lead to polymers with intriguing structures and interesting properties. In the coordination polymer catena-poly[[cadmium(II)-bis[μ-benzene-1,2-dicarboxylato-κ(4)O(1),O(1'):O(2),O(2')]-cadmium(II)-bis{μ-2-[(1H-imidazol-1-yl)methyl]-1H-benzimidazole}-κ(2)N(2):N(3);κ(2)N(3):N(2)] dimethylformamide disolvate], {[Cd(C8H4O4)(C11H10N4)]·C3H7NO}n, (I), each Cd(II) ion exhibits an irregular octahedral CdO4N2 coordination geometry and is coordinated by four O atoms from two symmetry-related benzene-1,2-dicarboxylate (1,2-bdic(2-)) ligands and two N atoms from two symmetry-related imb ligands. Two Cd(II) ions are connected by two benzene-1,2-dicarboxylate ligands to generate a binuclear [Cd2(1,2-bdic)2] unit. The binuclear units are further connected into a one-dimensional chain by pairs of bridging imb ligands. These one-dimensional chains are further connected through N-H...O hydrogen bonds and π-π interactions, leading to a two-dimensional layered structure. The dimethylformamide solvent molecules are organized in dimeric pairs via weak interactions. In addition, the title polymer exhibits good fluorescence properties in the solid state at room temperature.

  18. 2,3-二甲基-6-氨基-2H-吲唑的合成研究%A Study on the Synthesis of 2,3-diethyl-6-nitro-2H-indazole

    Institute of Scientific and Technical Information of China (English)

    刘兴赋; 傅晓钟; 吴忠世

    2010-01-01

    目的:设计与合成具有分子靶向性、低毒高效新型血管生成抑制剂类抗肿瘤药物中间体.方法:以2-乙基苯胺为原料经醋酐酰化、浓硝酸低温硝化及去酰基保护合成2-乙基-5-硝基苯胺,后用亚硝酸钠关环得3-甲基-6-硝基-1H-吲唑,经硫酸二甲酯甲基化得2,3-二甲基-6-硝基-2H-吲唑,最后用氯化亚锡将其还原得到目标产物,通过1H NMR确定结构与目标产物一致.结果:所用的合成方法可靠,质量可控,总收率为15.7%.结论:所采用合成方法能用于2,3-二甲基-6-氨基-2H-吲唑的制备.

  19. NMR spectroscopic properties (1H at 500 MHz) of deuterated* ribonucleotide-dimers ApU*, GpC*, partially deuterated 2'-deoxyribonucleotide-dimers d(TpA*), d(ApT*), d(GpC*) and their comparison with natural counterparts (1H-NMR window).

    Science.gov (United States)

    Földesi, A; Nilson, F P; Glemarec, C; Gioeli, C; Chattopadhyaya, J

    1993-02-01

    Pure 1'#,2',3',4'#,5',5''-2H6-ribonucleoside derivatives 10-14, 1'#,2',2'',3',4'#,5',5''-2H7-2'-deoxynucleoside blocks 15-18 and their natural-abundance counterparts were used to assemble partially deuterated ribonucleotide-dimers (* indicates deuteration at 1'#,2',3',4'#,5',5''(2H6)): ApU* 21, GpC* 22 and partially deuterated 2'-deoxyribonucleotide-dimers d(TpA*) 23, d(ApT*) 25, d(GpC*) 26 (* indicates deuteration at 1'#,2',2'',3',4'#,5',5''(2H7)) according to the procedure described by Földesi et al. (Tetrahedron, in press). These five partially deuterated oligonucleotides were subsequently compared with their corresponding natural-abundance counterparts by 500 MHz 1H-NMR spectroscopy to evaluate the actual NMR simplifications achieved in the non-deuterated part (1H-NMR window) as a result of specific deuterium incorporation. Detailed one-dimensional 1H-NMR (500 MHz), two-dimensional correlation spectra (DQF-COSY and TOCSY) and deuterium isotope effect on the chemical shifts of oligonucleotides have been presented.

  20. Synthesis of fatty trichloromethyl-{beta}-diketones and new 1H-Pyrazoles as unusual FAMEs and FAEEs

    Energy Technology Data Exchange (ETDEWEB)

    Flores, Alex F.C.; Souto, Alynne A.; Malavolta, Juliana L.; Flores, Darlene C., E-mail: alex.fcf@ufsm.br [Universidade Federal de Santa Maria (UFSM), RS (Brazil). Departamento de Quimica; Blanco, Rogerio F. [Uniao de Ensino do Sudoeste do Parana (UNISEP), Dois Vizinhos, PR (Brazil). Faculdade de Farmacia

    2013-12-01

    The efficient synthesis of new fatty 1,1,1-trichloro-4-methoxy-3-alken-2-ones [Cl{sub 3}CC(O)C(R{sup 2})=C(R{sup 1})OMe, where R{sup 1} = n-hexyl, heptyl, nonyl, undecyl, tridecyl and R{sup 2} = H] and 1,1,1-trichloro-2,4-alkanediones [Cl{sub 3}CC(O)CHR{sup 2}C(O)R{sup 1}, where R{sup 1} = n-pentyl and R{sup 2} = Me, R{sup 1} = Et and R{sup 2} = n-butyl, R{sup 1} = n-butyl and R{sup 2} = n-propyl] in good yields (85-95%) from acetal acylation with trichloroacetyl chloride is reported. The fatty 1,1,1-trichloro-4-methoxy-3-alken-2-ones and 1,1,1-trichloro-2,4-alkanediones were reacted with hydrazine hydrochloride, leading to respective {sup 1}H-pyrazole-5-carboxylates, unusual class of fatty acid methyl (FAMEs) and ethyl (FAEEs) esters. Their structures were confirmed by elemental analysis and {sup 1}H and {sup 13}C nuclear magnetic resonance (NMR). The fatty 1,1,1-trichloro-4-methoxy-3-alken-2-ones and {sup 1}H-pyrazole derivatives are new oleochemicals with potentially interesting and differential properties. (author)

  1. The Conformations and Structures of 1H-NONAFLUOROBUTANE

    Science.gov (United States)

    Fournier, Joseph A.; Bohn, Robert K.; Montgomery, John A.; , Jr.

    2012-06-01

    The all trans conformers of perfluorocarbons, unlike hydrocarbons, are helical with C-C-C-C dihedral angles about 1640. Fluorocarbons with H substitution can replace chlorofluorocarbons as propellants and compressor fluids without the disadvantage of causing ozone depletion in the upper atmosphere. 1H-perfluorobutane, CHF_2CF_2CF_2CF_3, has been studied by pulsed-jet Fourier transform microwave spectroscopy. The spectrum is very rich. Quantum chemical calculations identify five stable conformers with relative energies up to 1.1 kcal/mol. Thus far three conformers have been characterized and many lines remain unassigned. The assigned species have CCCCanti/CCCH gauche as well as the anti/anti and gauche/anti forms. Rotational constant values are 1428.9501(2) MHz, 593.323877(6) MHz, and 546.43578(6) MHz for the anti/gauche species, 1323.664(3) MHz, 617.6051(5) MHz for the ant/anti species, and 1066.9384(4) MHz, 768.4736(4) MHz, and 671.3145(4) MHz for the gauche/anti form.

  2. Tacrine derivatives-acetylcholinesterase interaction: 1H NMR relaxation study.

    Science.gov (United States)

    Delfini, Maurizio; Di Cocco, Maria Enrica; Piccioni, Fabiana; Porcelli, Fernando; Borioni, Anna; Rodomonte, Andrea; Del Giudice, Maria Rosaria

    2007-06-01

    Two acetylcholinesterase (AChE) inhibitors structurally related to Tacrine, 6-methoxytacrine (1a) and 9-heptylamino-6-methoxytacrine (1b), and their interaction with Electrophorus Electricus AChE were investigated. The complete assignment of the 1H and 13C NMR spectra of 1a and 1b was performed by mono-dimensional and homo- and hetero-correlated two-dimensional NMR experiments. This study was undertaken to elucidate the interaction modes between AChE and 1a and 1b in solution, using NMR. The interaction between the two inhibitors and AChE was studied by the analysis of the motional parameters non-selective and selective spin-lattice relaxation times, thereby allowing the motional state of 1a and 1b, both free and bound with AChE, to be defined. The relaxation data pointed out the ligands molecular moiety most involved in the binding with AChE. The relevant ligand/enzyme interaction constants were also evaluated for both compounds and resulted to be 859 and 5412M(-1) for 1a and1b, respectively.

  3. Mapping of prostate cancer by 1H MRSI.

    Science.gov (United States)

    Kobus, Thiele; Wright, Alan J; Scheenen, Tom W J; Heerschap, Arend

    2014-01-01

    In many studies, it has been demonstrated that (1)H MRSI of the human prostate has great potential to aid prostate cancer management, e.g. in the detection and localisation of cancer foci in the prostate or in the assessment of its aggressiveness. It is particularly powerful in combination with T2 -weighted MRI. Nevertheless, the technique is currently mainly used in a research setting. This review provides an overview of the state-of-the-art of three-dimensional MRSI, including the specific hardware required, dedicated data acquisition sequences and information on the spectral content with background on the MR-visible metabolites. In clinical practice, it is important that relevant MRSI results become available rapidly, reliably and in an easy digestible way. However, this functionality is currently not fully available for prostate MRSI, which is a major obstacle for routine use by inexperienced clinicians. Routine use requires more automation in the processing of raw data than is currently available. Therefore, we pay specific attention in this review on the status and prospects of the automated handling of prostate MRSI data, including quality control. The clinical potential of three-dimensional MRSI of the prostate is illustrated with literature examples on prostate cancer detection, its localisation in the prostate, its role in the assessment of cancer aggressiveness and in the selection and monitoring of therapy.

  4. Understanding Reverberation Lags in 1H0707-495

    CERN Document Server

    Zoghbi, A; Fabian, A C

    2010-01-01

    The first reverberation lag from the vicinity of a supermassive black hole was recently detected in the NLS1 galaxy 1H0707-495. We interpreted the lag as being due to reflection from matter close to the black hole, within a few gravitational radii of the event horizon (an inner reflector). It has since been claimed by Miller et al that the lag can be produced by more distant matter, at hundreds of gravitational radii (an outer reflector). Here, we critically explore their interpretation of the lag. The detailed energy dependence of the time lags between soft and hard energy bands is well modelled by an inner reflector using our previously published spectral model. A contrary claim by Miller et al was obtained by neglecting the blackbody component in the soft band. Soft lags can be produced by a large-scale outer reflector if several, implausible, conditions are met. An additional transfer function is required in the soft band corresponding to a region that is physically close to the continuum source, or lies ...

  5. The Structural Interface between HIV-1 Vif and Human APOBEC3H.

    Science.gov (United States)

    Ooms, Marcel; Letko, Michael; Simon, Viviana

    2017-03-01

    Human APOBEC3H (A3H) is a cytidine deaminase that inhibits HIV-1 replication. To evade this restriction, the HIV-1 Vif protein binds A3H and mediates its proteasomal degradation. To date, little information on the Vif-A3H interface has been available. To decipher how both proteins interact, we first mapped the Vif-binding site on A3H by functionally testing a large set of A3H mutants in single-cycle infectivity and replication assays. Our data show that the two A3H α-helixes α3 and α4 represent the Vif-binding site of A3H. We next used viral adaptation and a set of Vif mutants to identify novel, reciprocal Vif variants that rescued viral infectivity in the presence of two Vif-resistant A3H mutants. These A3H-Vif interaction points were used to generate the first A3H-Vif structure model, which revealed that the A3H helixes α3 and α4 interact with the Vif β-sheet (β2-β5). This model is in good agreement with previously reported Vif and A3H amino acids important for interaction. Based on the predicted A3H-Vif interface, we tested additional points of contact, which validated our model. Moreover, these experiments showed that the A3H and A3G binding sites on HIV-1 Vif are largely distinct, with both host proteins interacting with Vif β-strand 2. Taken together, this virus-host interface model explains previously reported data and will help to identify novel drug targets to combat HIV-1 infection.IMPORTANCE HIV-1 needs to overcome several intracellular restriction factors in order to replicate efficiently. The human APOBEC3 locus encodes seven proteins, of which A3D, A3F, A3G, and A3H restrict HIV-1. HIV encodes the Vif protein, which binds to the APOBEC3 proteins and leads to their proteasomal degradation. No HIV-1 Vif-APOBEC3 costructure exists to date despite extensive research. We and others previously generated HIV-1 Vif costructure models with A3G and A3F by mapping specific contact points between both proteins. Here, we applied a similar approach to HIV

  6. Novel bipyridinyl oxadiazole-based metal coordination complexes: High efficient and green synthesis of 3,4-dihydropyrimidin-2(1H)-ones through the Biginelli reactions

    Science.gov (United States)

    Wang, Jin-Hua; Zhang, E.; Tang, Gui-Mei; Wang, Yong-Tao; Cui, Yue-Zhi; Ng, Seik Weng

    2016-09-01

    Three new metal coordination complexes, namely, [Co(BPO)2(H2O)4](BS)2(H2O)2 (1), [Co(BPO)2(H2O)4](ABS)2(H2O)2 (2), [Co(BPO)2(H2O)4](MBS)2(H2O)2 (3) [BPO=2,5-di(pyridin-4-yl)-1,3,4-oxadiazole, BS=benzenesulphonate, ABS=4-aminobenzenesulphonate, MBS=4-methylbenzenesulphonate] were obtained under hydrothermal conditions. Complexes 1-3 were structurally characterized by single-crystal X-ray diffraction, powder X-ray diffraction, IR and thermogravimetric analyses (TGA). All of them display a zero-dimensional motif, in which strong intermolecular hydrogen bonding interactions (O-H···O/N) and packing interactions (C-H···π and π···π) make them achieve a three-dimensional supramolecular architecture. The primary catalytic results of these three complexes show that high efficiency for the green synthesis of a variety of 3,4-dihydropyrimidin-2(1H)-ones was observed under solvent free conditions through Biginelli reactions. The present catalytic protocols exhibit advantages such as excellent yield, easy isolation, eco-friendly conditions, and short reaction time.

  7. Modeling and validating tritium transfer in a grassland ecosystem in response to {sup 3}H releases

    Energy Technology Data Exchange (ETDEWEB)

    Le Dizes, S.; Maro, D.; Rozet, M.; Hebert, D.; Solier, L.; Nicoulaud, V. [Institut de radioportection et de surete nucleaire - IRSN (France); Vermorel, F.; Aulagnier, C. [Electricite de France - EDF (France)

    2014-07-01

    Tritium ({sup 3}H) is a major radionuclide released in several forms (HTO, HT) by nuclear facilities under normal operating conditions. In terrestrial ecosystems, tritium can be found under two forms: tritium in tissue free water (TFWT) following absorption of tritiated water by leaves or roots and Organically Bound Tritium (OBT) resulting from TFWT incorporation by the plant organic matter during photosynthesis. In order to study transfers of tritium from atmospheric releases to terrestrial ecosystem such as grasslands, an in-situ laboratory has been set up by IRSN on a ryegrass field plot located 2 km downwind the AREVA NC La Hague nuclear reprocessing plant (North-West of France), as was done in the past for the assessment of transfer of radiocarbon in grasslands. The objectives of this experimental field are: (i) to better understand the OBT formation in plant by photosynthesis, (ii) to evaluate transfer processes of tritium in several forms (HT, HTO) from the atmosphere (air and rainwater) to grass and soil, (iii) to develop a modeling allowing to reproduce the dynamic response of the ecosystem to tritium atmospheric releases depending of variable environmental conditions. For this purpose, tritium activity measurements will be carried out in grass (monthly measurements of HTO, OBT), in air, rainwater, soil (daily measurements of HT, HTO) and CO{sub 2}, H{sub 2}O fluxes between soil and air compartments will be carried out. Then, the TOCATTA-c model previously developed to simulate {sup 14}C transfers to pasture on a hourly time-step basis will be adapted to take account for processes specific to tritium. The model will be tested by a comparison between simulated results and measurements. The objectives of this presentation are (1) to present the organization of the experimental design of the VATO study (Validation of TOCATTA) dedicated to transfers of tritium in a grassland ecosystem, (2) to document the major assumptions, conceptual modelling and

  8. A facile synthesis and fungicidal activities of 2-(alkylamino-5,6-dimethylthieno[2,3-d]pyrimidin-4(3H-ones

    Directory of Open Access Journals (Sweden)

    2008-12-01

    Full Text Available The aza-Wittig reactions of iminophosphorane 3 with aromatic isocyanates generated carbodiimides 4, which were reacted with alkylamines under mild conditions to give a series of 2-(alkylamino-5,6-dimethylthieno[2,3-d]pyrimidin-4(3H-ones 6 and 8 in satisfactory yield. Their structures were confirmed by 1H NMR, EI-MS, IR and elementary analysis, and compound 8c was further analyzed by single-crystal X-ray diffraction. The preliminary bioassays indicated that these compounds showed excellent fungicidal activities against six kinds of fungi.

  9. Synthesis and characterization of two novel coordination polymers based on the rigid 1H-1,2,3-triazole-4,5-dicarboxylic acid ligand

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Two novel three-dimensional (3-D) coordination polymers, [Pb(HTDA)]n (1) and [Co5(TDA)2(H2TDA)2(H2O)8]n (2) [H3TDA = 1H-1,2,3-triazole-4,5-dicarboxylic acid], have been prepared by hydrothermal reactions and characterized by elemental analysis, infrared spectroscopy and single-crystal X-ray diffraction. Compound 1 is constructed from rod-shaped secondary building units (SBUs) and exhibits a 3-D network with (410·65)(410·63·82) topology. Compound 2 is built up from ligands bridging three different cobalt ions and exhibits a 3-D network with (4·82)3(4·82·103) topology. In addition, the thermal stabilities of the two compounds, the photoluminescence properties of compound 1 and the magnetic properties of compound 2 have been studied.

  10. Data of evolutionary structure change: 1JJIA-3H1BA [Confc[Archive

    Lifescience Database Archive (English)

    Full Text Available hain> 3H1BA WLLDQ----GFKPQ ...>HHH ---- > ATOM 942 CA TRP A 127 -20.677 16.86...Chain>1JJIA WVAENAEELRIDPS ture>HHHH HHHH ...3H1BA LNGAD-AKHPY >H - HH...ure> GGGGG HH> ATOM 1801 CA PHE A 223

  11. The abundance of C3H2 and other small hydrocarbons in the diffuse interstellar medium

    CERN Document Server

    Liszt, Harvey; Cordiner, Martin; Gerin, Maryvonne

    2012-01-01

    Hydrocarbons are ubiquitous in the interstellar medium, observed in diverse environments ranging from diffuse to molecular dark clouds and strong photon-dominated regions near HII regions. Recently, two broad diffuse interstellar bands (DIBs) at 4881{\\AA} and 5450{\\AA} were attributed to the linear version of propynylidene l-C3H2, a species whose more stable cyclic conformer c-C3H2 has been widely observed in the diffuse interstellar medium at radio wavelengths. This attribution has already been criticized on the basis of indirect plausibility arguments because the required column densities are quite large, N(l-C3H2)/EB-V = 4 \\times 1014 cm-2 mag-1. Here we present new measurements of N(l-C3H2) based on simultaneous 18-21 GHz VLA absorption profiles of cyclic and linear C3H2 taken along sightlines toward extragalactic radiocontinuum background sources with foreground Galactic reddening EB-V = 0.1 - 1.6 mag. We find that N(l-C3H2)/N(c-C3H2) ? 1/15 - 1/40 and N(l-C3H2)/EB-V ? 2 \\pm 1 \\times 1011 cm-2 mag-1, so ...

  12. Morphine enhances the release of /sup 3/H-purines from rat brain cerebral cortical prisms

    Energy Technology Data Exchange (ETDEWEB)

    Wu, P.H.; Phillis, J.W.; Yuen, H.

    1982-10-01

    In vitro experiments have shown that /sup 3/H-purines can be released from /sup 3/H-adenosine preloaded rat brain cortical prisms by a KCl-evoked depolarization. The KCl-evoked release of /sup 3/H-purines is dependent on the concentration of KCl present in the superfusate. At concentrations of 10(-7) approximately 10(-5)M morphine did not influence the basal release of /sup 3/H-purines from the prisms, although it enhanced the KCl-evoked release of /sup 3/H-purines. The enhancement of KCl-evoked /sup 3/H-purine release by morphine was concentration-dependent and was antagonized by naloxone, suggesting the involvement of opiate receptors. Uptake studies with rat brain cerebral cortical synaptosomes show that morphine is a very weak inhibitor of adenosine uptake. Comparisons with dipyridamole, a potent inhibitor of adenosine uptake, suggest that this low level of inhibition of the uptake did not contribute significantly to the release of /sup 3/H-purine by morphine seen in our experiments. It is therefore suggested that morphine enhances KCl-evoked /sup 3/H-purine release by an interaction with opiate receptors and that the resultant increase in extracellular purine (adenosine) levels may account for some of the actions of morphine.

  13. Nuclear accident-derived (3)H in river water of Fukushima Prefecture during 2011-2014.

    Science.gov (United States)

    Ueda, Shinji; Hasegawa, Hidenao; Kakiuchi, Hideki; Ochiai, Shinya; Akata, Naofumi; Hisamatsu, Shun'ichi

    2015-08-01

    During 2011-2014, we measured (3)H concentrations in river water samples collected during base flow conditions and during several flood events from two small rivers in a mountainous area in Fukushima Prefecture, which received deposition of (137)Cs from the Fukushima Dai-ichi Nuclear Power Plant accident. (3)H concentrations above background levels were found in water samples collected during both base flow conditions and flood events in 2011. The (3)H concentrations during flood events were generally higher than those during base flow conditions. The (3)H concentrations in both rivers during base flow conditions and flood events decreased with time after the accident and reached almost background levels in 2013. We also measured (3)H concentrations in freshwater samples from 16 other rivers and one dam in eastern Fukushima Prefecture from 2012 to 2014 during base flow conditions. The measured (3)H concentrations were higher than the background level in 2012 and decreased with time. The (137)Cs inventory in the catchment area at each sampling point was estimated from air-borne monitoring results in the literature and compared with the (3)H concentrations. We found surprisingly good correlations between (137)Cs inventories in the catchment areas and (3)H concentrations in the water samples. Further studies will be necessary to clarify the reason for the good correlation.

  14. Effect of hydroxyurea on mitotic activity 3H-thymidine and 3H-phenylalanine incorporation in the antheridial filament cells of Chara vulgaris

    Directory of Open Access Journals (Sweden)

    Anastazja Bilecka

    2015-01-01

    Full Text Available Hydroxyurea inhibits mitotic activity in cells of the antheridial filaments of Chara vulgaris by blocking phase S and phase G2. Blocking of cells in phase G2 also occurs in the case of the root meristem cells of Helianthus annuus and Vicia faba var. minor. 3H-thymidine incorporation confirmed autoradiographically the blocking of cells of the antheridial filaments in Chara vulgaris at phase S and slowing down of the rate of DNA replication. Incubation with 3H-phenylalanine demonstrated that hydroxyurea inhibits protein synthesis.

  15. A combined crossed beam and theoretical investigation of O(3P)+C3H3→C3H2+OH

    Science.gov (United States)

    Lee, Hohjai; Joo, Sun-Kyu; Kwon, Lee-Kyoung; Choi, Jong-Ho

    2004-02-01

    The radical-radical reaction dynamics of ground-state atomic oxygen [O(3P)] with propargyl radicals (C3H3) has first been investigated in a crossed beam configuration. The radical reactants O(3P) and C3H3 were produced by the photodissociation of NO2 and the supersonic flash pyrolysis of precursor propargyl bromide, respectively. A new exothermic channel of O(3P)+C3H3→C3H2+OH was identified and the nascent distributions of the product OH in the ground vibrational state (X 2Π:ν″=0) showed bimodal rotational excitations composed of the low- and high-N″ components without spin-orbit propensities. The averaged ratios of Π(A')/Π(A″) were determined to be 0.60±0.28. With the aid of ab initio theory it is predicted that on the lowest doublet potential energy surface, the reaction proceeds via the addition complexes formed through the barrierless addition of O(3P) to C3H3. The common direct abstraction pathway through a collinear geometry does not occur due to the high entrance barrier in our low collision energy regime. In addition, the major reaction channel is calculated to be the formation of propynal (CHCCHO)+H, and the counterpart C3H2 of the probed OH product in the title reaction is cyclopropenylidene (1c-C3H2) after considering the factors of barrier height, reaction enthalpy and structural features of the intermediates formed along the reaction coordinate. On the basis of the statistical prior and rotational surprisal analyses, the ratio of population partitioning for the low- and high-N″ is found to be about 1:2, and the reaction is described in terms of two competing addition-complex mechanisms: a major short-lived dynamic complex and a minor long-lived statistical complex. The observed unusual reaction mechanism stands in sharp contrast with the reaction of O(3P) with allyl radical (C3H5), a second significant conjugated hydrocarbon radical, which shows totally dynamic processes [J. Chem. Phys. 117, 2017 (2002)], and should be understood based

  16. Physical and spectroscopic properties of pure C2H4 and CH4:C2H4 ices

    Science.gov (United States)

    Molpeceres, Germán; Satorre, Miguel Angel; Ortigoso, Juan; Zanchet, Alexandre; Luna, Ramón; Millán, Carlos; Escribano, Rafael; Tanarro, Isabel; Herrero, Víctor J.; Maté, Belén

    2017-04-01

    Physical and spectroscopic properties of ices of C2H4 and CH4:C2H4 mixtures with 3:1, 1:1 and 1:3 ratios have been investigated at 30 K. Two laboratories are involved in this work. In one of them, the density and refractive index of the samples have been measured by using a cryogenic quartz microbalance and laser interferometric techniques. In the other one, IR spectra have been recorded in the near- and mid-infrared regions, and band shifts with respect to the pure species, band strengths of the main bands, and the optical constants in both regions have been determined. Previous data on ethylene and the mixtures studied here were scarce. For methane, both the wavenumbers and band strengths have been found to follow a regular pattern of decrease with increasing dilution, but no pattern has been detected for ethylene vibrations. The method employed for the preparation of the samples, by vapour deposition under vacuum, is thought to be adequate to mimic the structure of astrophysical ices. Possible astrophysical implications, especially by means of the optical constants reported here, have been discussed.

  17. 1H MAS and 1H --> 31P CP/MAS NMR study of human bone mineral.

    Science.gov (United States)

    Kaflak-Hachulska, A; Samoson, A; Kolodziejski, W

    2003-11-01

    Chemical structure of human bone mineral was studied by solid-state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS). Trabecular and cortical bone samples from adult subjects were compared with mineral standards: hydroxyapatite (HA), hydrated and calcined, carbonatoapatite of type B with 9 wt% of CO3(2-) (CHA-B), brushite (BRU) and mixtures of HA with BRU. Proton spectra were acquired with excellent spectral resolution provided by ultra-high speed MAS at 40 kHz. 2D 1H-31P NMR heteronuclear correlation was achieved by cross-polarization (CP) under fast MAS at 12 kHz. 31P NMR was applied with CP from protons under slow MAS at 1 kHz. Appearance of 31P rotational sidebands together with their CP kinetics were analyzed. It was suggested that the sidebands of CP spectra are particularly suitable for monitoring the state of apatite crystal surfaces. The bone samples appeared to be deficient in structural hydroxyl groups analogous to those in HA. We found no direct evidence that the HPO4(2-) brushite-like ions are present in bone mineral. The latter problem is extensively discussed in the literature. The study proves there is a similarity between CHA-B and bone mineral expressed by their similar NMR behavior.

  18. Vibrational and Rotational Spectroscopy of CD_2H^+

    Science.gov (United States)

    Asvany, Oskar; Jusko, Pavol; Brünken, Sandra; Schlemmer, Stephan

    2016-06-01

    The lowest rotational levels (J=0-5) of the CD_2H^+ ground state have been probed by high-resolution rovibrational and pure rotational spectroscopy in a cryogenic 22-pole ion trap. For this, the ν_1 rovibrational band has been revisited, detecting 107 transitions, among which 35 are new. The use of a frequency comb system allowed to measure the rovibrational transitions with high precision and accuracy, typically better than 1 MHz. The high precision has been confirmed by comparing combination differences in the ground and vibrationally excited state. For the ground state, this allowed for equally precise predictions of pure rotational transitions, 24 of which have been measured directly by a novel IR - mm-wave double resonance method. M.-F. Jagod et al, J. Molec. Spectrosc. 153, 666, 1992 S. Gartner et al, J. Phys. Chem. A 117, 9975, 2013

  19. 2H NMR studies of supercooled and glassy aspirin

    Science.gov (United States)

    Nath, R.; Nowaczyk, A.; Geil, B.; Bohmer, R.

    2007-11-01

    Acetyl salicylic acid, deuterated at the methyl group, was investigated using 2H-NMR in its supercooled and glassy states. Just above the glass transition temperature the molecular reorientations were studied using stimulated-echo spectroscopy and demonstrated a large degree of similarity with other glass formers. Deep in the glassy phase the NMR spectra look similar to those reported for the crystal [A. Detken, P. Focke, H. Zimmermann, U. Haeberlen, Z. Olejniczak, Z. T. Lalowicz, Z. Naturforsch. A 50 (1995) 95] and below 20 K they are indicative for rotational tunneling with a relatively large tunneling frequency. Measurements of the spin-lattice relaxation times for temperatures below 150 K reveal a broad distribution of correlation times in the glass. The dominant energy barrier characterizing the slow-down of the methyl group is significantly smaller than the well defined barrier in the crystal.

  20. Detailed Studies of Hydrocarbon Radicals: C2H Dissociation

    Energy Technology Data Exchange (ETDEWEB)

    Wittig, Curt

    2014-10-06

    A novel experimental technique was examined whose goal was the ejection of radical species into the gas phase from a platform (film) of cold non-reactive material. The underlying principle was one of photo-initiated heat release in a stratum that lies below a layer of CO2 or a layer of amorphous solid water (ASW) and CO2. A molecular precursor to the radical species of interest is deposited near or on the film's surface, where it can be photo-dissociated. It proved unfeasible to avoid the rampant formation of fissures, as opposed to large "flakes." This led to many interesting results, but resulted in our aborting the scheme as a means of launching cold C2H radical into the gas phase. A journal article resulted that is germane to astrophysics but not combustion chemistry.

  1. 2H and 18O Freshwater Isoscapes of Scotland

    Science.gov (United States)

    Meier-Augenstein, Wolfram; Hoogewerff, Jurian; Kemp, Helen; Frew, Danny

    2013-04-01

    Scotland's freshwater lochs and reservoirs provide a vital resource for sustaining biodiversity, agriculture, food production as well as for human consumption. Regular monitoring of freshwaters by the Scottish Environment Protection Agency (SEPA) fulfils legislative requirements with regards to water quality but new scientific methods involving stable isotope analysis present an opportunity combining these mandatory monitoring schemes with fundamental research to inform and deliver on current and nascent government policies [1] through gaining a greater understanding of Scottish waters and their importance in the context of climate change, environmental sustainability and food security. For example, 2H and 18O isoscapes of Scottish freshwater could be used to underpin research and its applications in: • Climate change - Using longitudinal changes in the characteristic isotope composition of freshwater lochs and reservoirs as proxy, isoscapes will provide a means to assess if and how changes in temperature and weather patterns might impact on precipitation patterns and amount. • Scottish branding - Location specific stable isotope signatures of Scottish freshwater have the potential to be used as a tool for provenancing and thus protecting premium Scottish produce such as Scottish beef, Scottish soft fruit and Scottish Whisky. During 2011 and 2012, with the support of SEPA more than 110 samples from freshwater lochs and reservoirs were collected from 127 different locations across Scotland including the Highlands and Islands. Here we present the results of this sampling and analysis exercise isotope analyses in form of 2H and 18O isoscapes with an unprecedented grid resolution of 26.5 × 26.5 km (or 16.4 × 16.4 miles). [1] Adaptation Framework - Adapting Our Ways: Managing Scotland's Climate Risk (2009): Scotland's Biodiversity: It's in Your Hands - A strategy for the conservation and enhancement of biodiversity in Scotland (2005); Recipe For Success - Scotland

  2. Study of morphology of aerosol aggregates formed during co-pyrolysis of C3H8 + Fe(CO)5

    Science.gov (United States)

    Ivanova, N. A.; Onischuk, A. A.; di Stasio, S.; Baklanov, A. M.; Makhov, G. A.

    2007-04-01

    Formation of aerosol nanoparticles as well as carbon nanotubes and nanofilaments is studied during co-pyrolysis of iron pentacarbonyl and propane with argon as a carrier gas in a flow reactor. Gaseous intermediates from propane thermal decomposition (CH4, C2H6 and C3H4) and Fe(CO)5 conversion are monitored by gas chromatography and IR-spectroscopy, respectively. The aerosol morphology is studied by transmission electron microscopy (TEM) and high resolution TEM. The aerosol particle concentration and size distribution are measured by an automated diffusion battery. The crystal phase composition of particles is studied by x-ray diffractometry. The decomposition of the Fe(CO)5 + Ar mixture resulted in an iron aggregate formation composed of fine primary particles. In the case of lower pyrolysis temperatures, about 450 K, the primary particle mean diameter is about 10 nm, and consequently, the majority of the primary particles are superparamagnetic, thus forming compact aggregates. At intermediate pyrolysis temperatures in the range 800-1040 K the primary particle diameter is about 20-30 nm, and most of the particles are ferromagnetic in nature. The coagulation of these particles results in a chain-like aggregate formation. Finally, at temperatures higher than the Curie point (1043 K) the ferromagnetic properties vanish and the formation of compact aggregates is observed again. The co-pyrolysis of Fe(CO)5 and C3H8 mixed with Ar carrier gas resulted in aerosol aggregate structures dramatically different from those formed by iron pentacarbonyl pyrolysis. In particular, in the temperature range 1070-1280 K, we observed Fe3C particles connected by long carbon nanotubes (CNTs). The aggregate morphology is described in terms of a fractal-like dimension Df, which is determined from TEM images on the basis of a scaling power law linking the aggregate mass (M) and radius (R), M{\\sim}R^{D_f} . The Fe3C-CNT aggregate morphology is a function of the inlet ratio between propane

  3. Crystal structure of 1H-imidazol-3-ium 2-(1,3-dioxoisoindolin-2-yl)acetate.

    Science.gov (United States)

    Mohamed, Shaaban K; Akkurt, Mehmet; Potgieter, Herman; Ali, Muizz

    2014-09-01

    The title salt, C3H5N2 (+)·C10H6NO4 (-), was obtained during a study of the co-crystallization of N'-[bis-(1H-imidazol-1-yl)methyl-ene]isonicotinohydrazide with (1,3-dioxoisoindolin-2-yl)acetic acid under aqueous conditions. The 1,3-dioxoisoindolinyl ring system of the anion is essentially planar [maximum deviation = 0.023 (2) Å]. In the crystal, cations and anions are linked via classical N-H⋯O hydrogen bonds and weak C-H⋯O hydrogen bonds, forming a three-dimensional network. Weak C-H⋯π inter-actions and π-π stacking inter-actions [centroid-centroid distances = 3.4728 (13) and 3.7339 (13) Å] also occur in the crystal.

  4. Accumulation of radioactivity after repeated infusion of 3H-adrenaline and 3H-noradrenaline in the rat as a model animal.

    Science.gov (United States)

    Lepschy, M; Filip, T; Palme, R G

    2014-10-01

    Besides enzymatic inactivation, catecholamines bind non-enzymatically and irreversible to proteins. The physiological impact of these catecholamine adducts is still unclear. We therefore collected basic data about the distribution of catecholamine adducts in the rat after repeated intravenous administration of (3)H-adrenaline and (3)H-noradrenaline. In all animals radioactivity in blood increased until the last injection on Day 7 and decreased then slowly close to background values (plasma) or remained higher (erythrocytes). In all sampled tissues radioactivity could be found, but only in hair high amounts remained present even after 3 weeks. Half-life of rat serum albumin loaded with (3)H-adrenaline or (3)H-noradrenaline was not altered. This study provides basic knowledge about the distribution of catecholamines or their adducts, but physiological effects could not be demonstrated. However, for the first time deposition and accumulation of catecholamines (adducts) in the hair could be proven, suggesting that hair might be used for evaluating long term stress.

  5. Anomalous absorption in c-C_3H and c-C_3D radicals

    Science.gov (United States)

    Chandra, S.; Shinde, S. V.; Kegel, W. H.; Sedlmayr, E.

    Yamamoto et al. (1987) reported the first detection of the c-C_3H radical in TMC-1 through its transition 2_1 2 rightarrow 1_1 1 at 91.5 GHz. The column density of c-C_3H in TMC-1 was estimated to be 6 times 10^12 cm^-2, which is about one order of magnitude lower than that of the c-C_3H_2 which is ubiquitous in galactic objects. Mangum & Wootten (1990) detected c-C_3H through the transition 1_1 0 rightarrow 1_1 1 at 14.8 GHz in 12 additional galactic objects. The most probable production mechanism of both the c-C_3H and c-C_3H_2 in dark clouds is a common dissociation reaction of the C_3H_3^+ ion (Adams & Smith 1987). Although the c-C_3H is 0.8 eV less stable than its isomer l-C_3H, finding of comparable column densities of both the isomers in TMC-1 suggests that the formation rate for both, c-C_3H and l-C_3H, are of about the same order in the cosmic objects. The existence of a metastable isomer under interstellar conditions is a well known phenomenon in astronomy. The aim of this investigation is a quantitative estimate of relative line intensities under NLTE conditions. For wide ranges of physical parameters, where these molecules may be found, we have solved a set of statistical equilibrium equations coupled with the equations of radiative transfer in an on-the-spot approximation. For c-C_3H, we accounted for 51 energy levels connected by 207 radiative transitions and for c-C_3D, we accounted for 51 energy levels connected by 205 radiative transitions. Our results show that the 3_3 1 rightarrow 3_3 0 transition of c-C_3H and c-C_3D may be found in absorption against the cosmic microwave background (CMB). Furthermore, we found population inversion for the 1_1 0 rightarrow 1_1 1 transition. These findings may be useful in identifying these molecules in other cosmic objects, as well as for the determination of physical parameters in these objects.

  6. A validation of the 3H/3He method for determining groundwater recharge

    Science.gov (United States)

    Solomon, D. K.; Schiff, S. L.; Poreda, R. J.; Clarke, W. B.

    1993-09-01

    Tritium and He isotopes have been measured at a site where groundwater flow is nearly vertical for a travel time of 100 years and where recharge rates are spatially variable. Because the mid-1960s 3H peak (arising from aboveground testing of thermonuclear devices) is well-defined, the vertical groundwater velocity is known with unusual accuracy at this site. Utilizing 3H and its stable daughter 3He to determine groundwater ages, we compute a recharge rate of 0.16 m/yr, which agrees to within about 5% of the value based on the depth of the 3H peak (measured both in 1986 and 1991) and two-dimensional modeling in an area of high recharge. Zero 3H/3He age occurs at a depth that is approximately equal to the average depth of the annual low water table, even though the capillary fringe extends to land surface during most of the year at the study site. In an area of low recharge (0.05 m/yr) where the 3H peak (and hence the vertical velocity) is also well-defined, the 3H/3He results could not be used to compute recharge because samples were not collected sufficiently far above the 3H peak; however, modeling indicates that the 3H/3He age gradient near the water table is an accurate measure of vertical velocities in the low-recharge area. Because 3H and 3He have different diffusion coefficients, and because the amount of mechanical mixing is different in the area of high recharge than in the low-recharge area, we have separated the dispersive effects of mechanical mixing from molecular diffusion. We estimate a longitudinal dispersivity of 0.07 m and effective diffusion coefficients for 3H (3HHO) and 3He of 2.4×10-5 and 1.3×10-4 m2/day, respectively. Although the 3H/3He age gradient is an excellent indicator of vertical groundwater velocities above the mid-1960s 3H peak, dispersive mixing and diffusive loss of 3He perturb the age gradient near and below the 3H peak.

  7. 298 K rate coefficients for the reaction of OH with i-C3H7I, n-C3H7I and C3H8

    Directory of Open Access Journals (Sweden)

    J. N. Crowley

    2001-09-01

    Full Text Available The kinetics of the title reactions were investigated using the laser photolysis - resonance fluorescence method, employing the sequential two-photon dissociation of NO2 in the presence of H2 as the OH source. The 298 K rate constant for OH + C3H8 was found to be (1.15±0.1 × 10-12 cm3 s-1, in excellent agreement with the literature recommendation, and with a separate determination using HNO3 photolysis at 248 nm as the OH source. The 298 K rate constants for OH + n-C3H7I and i-C3H7I were measured for the first time and found to be (1.47±0.08 and (1.22±0.06 × 10-12 cm3 s-1, respectively. The errors include an assessment of systematic error due to concentration measurement, which, for the propyl-iodides was minimised by on-line UV-absorption spectroscopy. The implications of these results for the reactive iodine budget of the marine boundary layer are discussed.

  8. Complete {sup 1}H and {sup 13}C NMR assignments of isojuripidine from Solanum asterophorum Mart

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Tania M.S.; Costa, Rodrigo A.; Oliveira, Eduardo J.; Barbosa-Filho, Jose M.; Agra, Maria F.; Camara, Celso A. [Universidade Federal da Paraiba, Joao Pessoa, PB (Brazil). Lab. de Tecnologia Farmaceutica]. E-mail: sarmento@ltf.ufpb.br

    2005-11-15

    Isojuripidine was isolated from the aerial parts of Solanum astherophorum Mart. Its structure was determined using a combination of homo- (1D {sup 1}H NMR, {sup 13}C NMR-HBBD and {sup 13}C NMRDEPT) and heteronuclear 2D NMR techniques ({sup 1}H-{sup 1}H-COSY, {sup 1}H-{sup 1}H-NOESY, HSQC, HMBC), and HREIMS. The unambiguous assignments of {sup 1}H and {sup 13}C NMR data of derivatives 3-N,6-Odiacetyl- isojuripidine and 3-N-cinnamoyl-isojuripidine are described. (author)

  9. Dopaminergic 3H-agonist receptors in rat brain: new evidence on localization and pharmacology

    Energy Technology Data Exchange (ETDEWEB)

    Bacopoulos, N.G.

    1984-01-23

    Recent methodological advances have allowed the reliable assay of specific dopaminergic 3H-agonist binding sites in rat striatum. Lesions of dopamine(DA) terminals or drugs which deplete DA levels prevent the preincubation-induced increase in binding, and this effect is completely reversible by preincubation with added DA. It is concluded that the evidence supporting the existence of presynaptic D-3 sites is artefactual and that 3H-DA binding sites are more likely related to post-synaptic receptors. 3H-DA binding involves two sites, one of which has pharmacologic properties similar to D-1 receptors, whereas the other resembles D-2 receptors. The affinity of 15 antipsychotic drugs for 3H-haloperidol binding sites was highly correlated (R = 0.94) with their inhibitory potency at a subset of 3H-DA binding sites. However, the inhibition of 3H-DA binding by antipsychotic drugs was noncompetitive. These findings can be explained by an allosteric model, whereby antagonists bind to a site different from but allosterically linked to a high-affinity 3H-DA binding site.

  10. [3H]ATPA: a high affinity ligand for GluR5 kainate receptors.

    Science.gov (United States)

    Hoo, K; Legutko, B; Rizkalla, G; Deverill, M; Hawes, C R; Ellis, G J; Stensbol, T B; Krogsgaard-Larsen, P; Skolnick, P; Bleakman, D

    1999-12-01

    The pharmacological properties of [3H]ATPA ((RS)-2-amino-3(3-hydroxy-5-tert-butylisoxazol-4-yl)propanoic acid) are described. ATPA is a tert-butyl analogue of AMPA (alpha-amino-3-hydroxy-5-methyl-4-isoxazoleproprionic acid) that has been shown to possess high affinity for the GluR5 subunit of kainate receptors. [3H]ATPA exhibits saturable, high affinity binding to membranes expressing human GluR5 (GluR5) kainate receptors (Kd approximately 13 nM). No specific binding was observed in membranes expressing GluR2 and GluR6 receptors. Several compounds known to interact with the GluR5 kainate receptor inhibited [3H]ATPA binding with potencies similar to those obtained for competition of [3H]kainate binding to GluR5. Saturable, high affinity [3H]ATPA binding (Kd approximately 4 nM) was also observed in DRG neuron (DRG) membranes isolated from neonatal rats. The rank order potency of compounds to inhibit [3H]ATPA binding in rat DRG and GluR5 membranes were in agreement. These finding demonstrate that [3H]ATPA can be used as a radioligand to examine the pharmacological properties of GluR5 containing kainate receptors.

  11. High affinity binding of (/sup 3/H)cocaine to rat liver microsomes

    Energy Technology Data Exchange (ETDEWEB)

    El-Maghrabi, E.A.; Calligaro, D.O.; Eldefrawi, M.E.

    1988-01-01

    )/sup 3/H)cocaine bound reversible, with high affinity and stereospecificity to rat liver microsomes. Little binding was detected in the lysosomal, mitochondrial and nuclear fractions. The binding kinetics were slow and the kinetically calculated K/sub D/ was 2 nM. Induction of mixed function oxidases by phenobarbital did not produce significant change in (/sup 3/H)cocaine binding. On the other hand, chronic administration of cocaine reduced (/sup 3/H)cocaine binding drastically. Neither treatment affected the affinity of the liver binding protein for cocaine. Microsomes from mouse and human livers had less cocaine-binding protein and lower affinity for cocaine than those from rat liver. Binding of (/sup 3/H)cocaine to rat liver microsomes was insensitive to monovalent cations and > 10 fold less sensitive to biogenic amines than the cocaine receptor in rat striatum. However, the liver protein had higher affinity for cocaine and metabolites except for norcocaine. Amine uptake inhibitors displaced (/sup 3/H)cocaine binding to liver with a different rank order of potency than their displacement of (/sup 3/H)cocaine binding to striatum. This high affinity (/sup 3/H)cocaine binding protein in liver is not likely to be monooxygenase, but may have a role in cocaine-induced hepatotoxicity

  12. ( sup 3 H)cytisine binding to nicotinic cholinergic receptors in brain

    Energy Technology Data Exchange (ETDEWEB)

    Pabreza, L.A.; Dhawan, S.; Kellar, K.J. (Georgetown Univ. School of Medicine, Washington, DC (USA))

    1991-01-01

    Cytisine, a ganglionic agonist, competes with high affinity for brain nicotinic cholinergic receptors labeled by any of several nicotinic {sup 3}H-agonist ligands. Here we have examined the binding of ({sup 3}H)cytisine in rat brain homogenates. ({sup 3}H)Cytisine binds with high affinity (Kd less than 1 nM), and specific binding represented 60-90% of total binding at all concentrations examined up to 15 nM. The nicotinic cholinergic agonists nicotine, acetylcholine, and carbachol compete with high affinity for ({sup 3}H)cytisine binding sites, whereas among nicotinic receptor antagonists only dihydro-beta-erythroidine competes with high affinity (in the nanomolar range). Comparison of binding in several brain regions showed that ({sup 3}H)cytisine binding is higher in the thalamus, striatum, and cortex than in the hippocampus, cerebellum, or hypothalamus. The pharmacology and brain regional distribution of ({sup 3}H)cytisine binding sites are those predicted for neuronal nicotinic receptor agonist recognition sites. The high affinity and low nonspecific binding of ({sup 3}H)cytisine should make it a very useful ligand for studying neuronal nicotinic receptors.

  13. [3H]WIN 35,065-2: a ligand for cocaine receptors in striatum.

    Science.gov (United States)

    Ritz, M C; Boja, J W; Grigoriadis, D; Zaczek, R; Carroll, F I; Lewis, A H; Kuhar, M J

    1990-11-01

    [3H]WIN 35,065-2 binding to striatal membranes was characterized, primarily by centrifugation assay. Like [3H]cocaine, [3H]WIN 35,065-2 binds to both high- and low-affinity sites. [3H]WIN 35,065-2, however, exhibits consistently higher affinities than [3H]cocaine. Saturation experiments indicate a low-affinity binding site with an apparent KD of approximately 160 nM and a Bmax of 135 fmol/mg of tissue. A high-affinity site has also been identified with an apparent KD of 5.6 nM and a Bmax of 5.2 fmol/mg of tissue. The specific-to-nonspecific binding ratios with [3H]WIN 35,065-2 were higher than with [3H]cocaine in both centrifugation and filtration assays. Pharmacological characterization suggests that [3H]WIN 35,065-2 binds to the dopamine transporter. Mazindol, GBR 12909, nomifensine, and (-)-cocaine are potent inhibitors of [3H]WIN 35,065-2 binding. In contrast, the norepinephrine transporter ligand desipramine is a weak inhibitor, and the serotonin transporter ligand citalopram does not inhibit binding. The effect of sodium on binding was examined under conditions in which (a) the low-affinity site was primarily (87%) occupied and (b) approximately 50% of both sites were occupied. The results indicate that both sites are sodium dependent. Injection of 6-hydroxydopamine into the striatum results in a significant loss of both high- and low-affinity sites, a finding suggesting that both sites are on dopaminergic nerve terminals. Taken together, these data are consistent with the presence of multiple cocaine binding sites associated with the dopamine transporter.

  14. Measurement of {sup 1}H-{sup 15}N and {sup 1}H-{sup 13}C residual dipolar couplings in nucleic acids from TROSY intensities

    Energy Technology Data Exchange (ETDEWEB)

    Ying Jinfa [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Wang Jinbu [National Cancer Institute, National Institutes of Health, Structural Biophysics Laboratory (United States); Grishaev, Alex [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Yu Ping; Wang Yunxing [National Cancer Institute, National Institutes of Health, Structural Biophysics Laboratory (United States); Bax, Ad, E-mail: bax@nih.gov [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States)

    2011-09-15

    Analogous to the recently introduced ARTSY method for measurement of one-bond {sup 1}H-{sup 15}N residual dipolar couplings (RDCs) in large perdeuterated proteins, we introduce methods for measurement of base {sup 13}C-{sup 1}H and {sup 15}N-{sup 1}H RDCs in protonated nucleic acids. Measurements are based on quantitative analysis of intensities in {sup 1}H-{sup 15}N and {sup 13}C-{sup 1}H TROSY-HSQC spectra, and are illustrated for a 71-nucleotide adenine riboswitch. Results compare favorably with those of conventional frequency-based measurements in terms of completeness and convenience of use. The ARTSY method derives the size of the coupling from the ratio of intensities observed in two TROSY-HSQC spectra recorded with different dephasing delays, thereby minimizing potential resonance overlap problems. Precision of the RDC measurements is limited by the signal-to-noise ratio, S/N, achievable in the 2D TROSY-HSQC reference spectrum, and is approximately given by 30/(S/N) Hz for {sup 15}N-{sup 1}H and 65/(S/N) Hz for {sup 13}C-{sup 1}H. The signal-to-noise ratio of both {sup 1}H-{sup 15}N and {sup 1}H-{sup 13}C spectra greatly benefits when water magnetization during the experiments is not perturbed, such that rapid magnetization transfer from bulk water to the nucleic acid, mediated by rapid amino and hydroxyl hydrogen exchange coupled with {sup 1}H-{sup 1}H NOE transfer, allows for fast repetition of the experiment. RDCs in the mutated helix 1 of the riboswitch are compatible with nucleotide-specifically modeled, idealized A-form geometry and a static orientation relative to the helix 2/3 pair, which differs by ca 6 Degree-Sign relative to the X-ray structure of the native riboswitch.

  15. Sublingual versus vaginal misoprostol for cervical dilatation 1 or 3 h prior to surgical abortion: a double-blinded RCT.

    Science.gov (United States)

    Sääv, Ingrid; Kopp Kallner, Helena; Fiala, Christian; Gemzell-Danielsson, Kristina

    2015-06-01

    Can sublingual administration of misoprostol 1 h prior to vacuum aspiration be more effective than vaginal administration and as effective as either route three 3 h prior to surgery? Sublingually administered misoprostol is superior to vaginally administered misoprostol when given 1 h pre operatively, and it is as effective as after a three 3 h priming interval with either route of administration. Misoprostol reduces complications and morbidity when used for cervical priming prior to surgical dilatation and vacuum aspiration in first trimester pregnancy. Despite the widespread use and extensive studies, the optimal route of administration of misoprostol before surgical abortion remains to be defined. The optimal priming interval after vaginal and sublingual administration of 400 mcg misoprostol has been reported to be 3 h. A longer interval will not improve dilatation but will increase the risk for bleeding and expulsion of the uterine contents before surgical evacuation. The pharmacokinetic properties of misoprostol indicate that sublingual compared with vaginal administration of misoprostol may result in a more rapid cervical priming effect. Women were randomized to four treatment groups and received 400 mcg misoprostol sublingually, or vaginally, 1 or 3 h prior to surgery. The study was a double-blinded RCT with regard to route of misoprostol administration but not the timing interval. The primary outcome was baseline cervical dilatation after misoprostol priming. The study was conducted between June 2007 and March 2014 and 184 women aged 18 years or older were recruited. Women were recruited among nulliparous women undergoing elective surgical first trimester abortion. Exclusion criteria were any contraindication for misoprostol, untreated genital infection, previous history of surgery to the cervix, or abnormal pregnancy. Gestational age was established by endovaginal ultrasound examination. The trial was conducted in a university hospital outpatient clinic

  16. Synthesis of Some Novel 2,6-Disubstituted Pyridazin-3(2H)-one Derivatives as Analgesic, Anti-Inflammatory, and Non-Ulcerogenic Agents.

    Science.gov (United States)

    Ibrahim, Tamer H; Loksha, Yasser M; Elshihawy, Hosam A; Khodeer, Dina M; Said, Mohamed M

    2017-09-01

    Some novel 2,6-disubstituted pyridazine-3(2H)-one derivatives were synthesized and evaluated for in vitro cyclooxygenase-2 (COX-2) inhibitory efficacy. Compounds 2-{[3-(2-methylphenoxy)-6-oxopyridazin-1(6H)-yl]methyl}-1H-isoindole-1,3(2H)-dione (5a), 2-propyl-6-(o-tolyloxy)pyridazin-3(2H)-one (6a), and 2-benzyl-6-(3,5-dimethyl-1H-pyrazol-1-yl)pyridazin-3(2H)-one (16a) showed the most potent COX-2 inhibitory activity with IC50 values of 0.19, 0.11, and 0.24 μM, respectively. The synthesized compounds with the highest COX-2 selectivity indices were evaluated for their anti-inflammatory, analgesic, and ulcerogenic activities. Compounds 6a and 16a demonstrated the most potent and consistent anti-inflammatory activity over the synthesized compounds, which was significantly higher than that of celecoxib in the carrageenin rat paw edema model and with milder ulcer scoring than that of indomethacin in the ulcerogenicity screening. © 2017 Deutsche Pharmazeutische Gesellschaft.

  17. Increased binding of [3H]GABA to striatal membranes following ischemia.

    Science.gov (United States)

    Francis, A; Pulsinelli, W

    1983-05-01

    Sodium-independent binding of [3H]gamma-aminobutyric acid ([3H]GABA) to membranes prepared from ischemic-damaged rat striatum was studied by kinetic and time-course analysis. Three days after 40 min of ischemia, [3H]GABA binding increased fourfold over control values. Scatchard analysis of the binding showed that ischemia significantly increased the affinity (KD) and the total number of binding sites (Bmax) for the high-affinity GABA receptor. These results support the conclusion that transient forebrain ischemia damages striatal GABAergic neurons.

  18. The synthesis of (4- sup 3 H)oxiracetam - a novel nootropic agent

    Energy Technology Data Exchange (ETDEWEB)

    Crowe, A.M.; Lawrie, K.W.M.; Saunders, D. (SmithKline Beecham Pharmaceuticals, Welwyn (UK)); Pfeiffer, U. (ISF, Milan (Italy))

    1991-01-01

    The synthesis of (4-{sup 3}H)oxiracetam from ethyl 2-(4-chloro-3-oxo-butyramido)acetate is described. Ethyl 2-(4-chloro-3-oxo-butyramido)-acetate was reduced with sodium borotritide at Amersham International plc to give ethyl 2-(4-chloro-(3-{sup 3}H)-3-hydroxy-butyramido)acetate. This was elaborated, in four steps, to (4-{sup 3}H)oxiracetam in 4.8% overall radiochemical yield, furnishing 5735 {mu}Ci, 212 MBq, 41.8 {mu}g, of specific activity 21.7 Ci/mmol, 802.9 GBq/mmol, and radiochemical purity of greater than 98%. (author).

  19. Facile synthesis of 1-alkoxy-1H-benzo- and 7-azabenzotriazoles from peptide coupling agents, mechanistic studies, and synthetic applications

    Directory of Open Access Journals (Sweden)

    Mahesh K. Lakshman

    2014-08-01

    Full Text Available (1H-Benzo[d][1,2,3]triazol-1-yloxytris(dimethylaminophosphonium hexafluorophosphate (BOP, 1H-benzo[d][1,2,3]triazol-1-yl 4-methylbenzenesulfonate (Bt-OTs, and 3H-[1,2,3]triazolo[4,5-b]pyridine-3-yl 4-methylbenzenesulfonate (At-OTs are classically utilized in peptide synthesis for amide-bond formation. However, a previously undescribed reaction of these compounds with alcohols in the presence of a base, leads to 1-alkoxy-1H-benzo- (Bt-OR and 7-azabenzotriazoles (At-OR. Although BOP undergoes reactions with alcohols to furnish 1-alkoxy-1H-benzotriazoles, Bt-OTs proved to be superior. Both, primary and secondary alcohols undergo reaction under generally mild reaction conditions. Correspondingly, 1-alkoxy-1H-7-azabenzotriazoles were synthesized from At-OTs. Mechanistically, there are three pathways by which these peptide-coupling agents can react with alcohols. From 31P{1H}, [18O]-labeling, and other chemical experiments, phosphonium and tosylate derivatives of alcohols seem to be intermediates. These then react with BtO− and AtO− produced in situ. In order to demonstrate broader utility, this novel reaction has been used to prepare a series of acyclic nucleoside-like compounds. Because BtO− is a nucleofuge, several Bt-OCH2Ar substrates have been evaluated in nucleophilic substitution reactions. Finally, the possible formation of Pd π–allyl complexes by departure of BtO− has been queried. Thus, alpha-allylation of three cyclic ketones was evaluated with 1-(cinnamyloxy-1H-benzo[d][1,2,3]triazole, via in situ formation of pyrrolidine enamines and Pd catalysis.

  20. Synthesis of 1H-indazoles and 1H-pyrazoles via FeBr3/O2 mediated intramolecular C-H amination.

    Science.gov (United States)

    Zhang, Tianshui; Bao, Weiliang

    2013-02-01

    A new synthesis of substituted 1H-indazoles and 1H-pyrazoles from arylhydrazones via FeBr(3)/O(2) mediated C-H activation/C-N bond formation reactions is reported. The corresponding 1,3-diaryl-substituted indazoles and trisubstituted pyrazoles were obtained in moderate to excellent yields under mild conditions.

  1. Description and validation of a rapid (1 h) flow cytometry test for enumerating thermophilic bacteria in milk powders.

    Science.gov (United States)

    Flint, S; Walker, K; Waters, B; Crawford, R

    2007-04-01

    The aim of this study was to develop a rapid assay for enumerating thermophilic bacteria in milk powder. The BactiFlow flow cytometer was used to count bacteria based on esterase activity in viable bacterial cells. A protocol for total viable bacteria was modified by heat-treating the sample to selectively label thermophilic bacteria. Samples of milk powder dissolved in 0.1% peptone were treated with 0.8% ethylenediaminetetraacetic acid to reduce background interference because of denatured milk proteins. Either thermophilic bacteria were added to the dissolved milk powder or milk powder solutions were incubated at 55 degrees C for 2-3 h to enrich the natural thermophile population for testing. Results from the BactiFlow were compared with traditional plate count results. Thermophilic bacteria in milk powder can be enumerated within 1 h using the BactiFlow flow cytometer. Microbiological test results obtained within 1 h can potentially be used to monitor manufacturing processes, effectively trace problems and provide confidence in the manufacture of product.

  2. Crystal structure of trans-diaquabis(1H-pyrazole-3-carboxylato-κ2N,Ocopper(II dihydrate

    Directory of Open Access Journals (Sweden)

    Santiago Reinoso

    2015-12-01

    Full Text Available In the title compound, [Cu(C4H3N2O22(H2O2]·2H2O, the CuII ion is located on an inversion centre and exhibits an axially elongated octahedral coordination geometry. The equatorial plane is formed by two N,O-bidentate 1H-pyrazole-3-carboxylate ligands in a trans configuration. The axial positions are occupied by two water molecules. The mononuclear complex molecules are arranged in layers parallel to the ab plane. Each complex molecule is linked to four adjacent species through intermolecular O—H...O and N—H...O hydrogen bonds that are established between the coordinating water molecules and carboxylate O atoms or protonated N atoms of the organic ligands. These layers are further connected into a three-dimensional network by additional hydrogen bonds involving solvent water molecules and non-coordinating carboxylate O atoms.

  3. Diaqua-(5-methyl-1H-pyrazole-3-carboxyl-ato)(4-nitro-benzoato)copper(II).

    Science.gov (United States)

    Hu, Fei-Long; Yin, Xian-Hong; Feng, Yu; Mi, Yan; Zhang, Shan-Shan

    2009-01-23

    In the title complex, [Cu(C(7)H(4)NO(4))(C(5)H(5)N(2)O(2))(H(2)O)(2)], the Cu(II) ion is coordinated in a slightly distorted square-pyramidal enviroment. The basal plane is formed by an N atom and an O atom from a 5-methyl-1H-pyrazole-3-carboxyl-ate ligand and by two O atoms from two water ligands. The apical position is occupied by a carboxylate O atom from a 4-nitro-benzoate ligand. In the crystal structure, inter-molecular O-H⋯O and N-H⋯O hydrogen bonds link complex moleclues, forming extended chains parallel to the a axis.

  4. On the Formation of the C2H6O Isomers Ethanol (C2H5OH) and Dimethyl Ether (CH3OCH3) in Star-forming Regions

    Science.gov (United States)

    Bergantini, Alexandre; Maksyutenko, Pavlo; Kaiser, Ralf I.

    2017-06-01

    The structural isomers ethanol (CH3CH2OH) and dimethyl ether (CH3OCH3) were detected in several low-, intermediate-, and high-mass star-forming regions, including Sgr B2, Orion, and W33A, with the relative abundance ratios of ethanol/dimethyl ether varying from about 0.03 to 3.4. Until now, no experimental data regarding the formation mechanisms and branching ratios of these two species in laboratory simulation experiments could be provided. Here, we exploit tunable photoionization reflectron time-of-flight mass spectrometry (PI-ReTOF-MS) to detect and analyze the production of complex organic molecules (COMs) resulting from the exposure of water/methane (H2O/CH4) ices to energetic electrons. The main goal is to understand the formation mechanisms in star-forming regions of two C2H6O isomers: ethanol (CH3CH2OH) and dimethyl ether (CH3OCH3). The results show that the experimental branching ratios favor the synthesis of ethanol versus dimethyl ether (31 ± 11:1). This finding diverges from the abundances observed toward most star-forming regions, suggesting that production routes on interstellar grains to form dimethyl ether might be missing; alternatively, ethanol can be overproduced in the present simulation experiments, such as via radical-radical recombination pathways involving ethyl and hydroxyl radicals. Finally, the PI-ReTOF-MS data suggest the formation of methylacetylene (C3H4), ketene (CH2CO), propene (C3H6), vinyl alcohol (CH2CHOH), acetaldehyde (CH3CHO), and methyl hydroperoxide (CH3OOH), in addition to ethane (C2H6), methanol (CH3OH), and CO2 detected from infrared spectroscopy. The yield of all the confirmed species is also determined.

  5. [Preparation of Di3H(9,10)-hydroergot Alkaloids (author's transl)].

    Science.gov (United States)

    Riedel, E; Roetz, R; Nündel, M

    1978-01-01

    In katalytic hydrogenation of native ergot alkaloids with tritium a specific addition of 3H in 9,10 position of the molecules results. The most favourable technique is described in detail on the example of ergotamine/dihydroergotamine.

  6. Ground state structures and properties of Si3H ( = 1–6) clusters

    Indian Academy of Sciences (India)

    D Balamurugan; R Prasad

    2003-01-01

    The ground state structures and properties of Si3H (1 ≤ ≤ 6) clusters have been calculated using Car–Parrinello molecular dynamics with simulated annealing and steepest descent optimization methods. We have studied cohesive energy per particle and first excited electronic level gap of the clusters as a function of hydrogenation. Hydrogenation is done till all dangling bonds of silicon are saturated. Our results show that over coordination of hydrogen is favoured in Si3H clusters and the geometry of Si3 cluster does not change due to hydrogenation. Cohesive energy per particle and first excited electronic level gap study of the clusters show that Si3H6 cluster is most stable and Si3H3 cluster is most unstable among the clusters considered here.

  7. Alpha 2 adrenergic receptors in hyperplastic human prostate: identification and characterization using (/sup 3/H) rauwolscine

    Energy Technology Data Exchange (ETDEWEB)

    Shapiro, E.; Lepor, H.

    1986-05-01

    (/sup 3/H)Rauwolscine ((/sup 3/H)Ra), a selective ligand for the alpha 2 adrenergic receptor, was used to identify and characterize alpha 2 adrenergic receptors in prostate glands of men with benign prostatic hyperplasia. Specific binding of (/sup 3/H)Ra to prostatic tissue homogenates was rapid and readily reversible by addition of excess unlabelled phentolamine. Scatchard analysis of saturation experiments demonstrates a single, saturable class of high affinity binding sites (Bmax = 0.31 +/- 0.04 fmol./microgram. DNA, Kd = 0.9 +/- 0.11 nM.). The relative potency of alpha adrenergic drugs (clonidine, alpha-methylnorepinephrine and prazosin) in competing for (/sup 3/H)Ra binding sites was consistent with the order predicted for an alpha 2 subtype. The role of alpha 2 adrenergic receptors in normal prostatic function and in men with bladder outlet obstruction secondary to BPH requires further investigation.

  8. Placental transfer and fetal distribution of /sup 3/H-retinoic acid in rats

    Energy Technology Data Exchange (ETDEWEB)

    Shukla, R.R.; Kumar, V.; Banerjee, R.; Misra, U.K.

    1986-01-01

    The placental transfer of /sup 3/H-retinoic acid in vitamin A deprived and vitamin A supplemented pregnant female rats was studied on 20th day of gestation and compared with /sup 3/H-retinyl acetate. Radiolabelled compounds were administered to pregnant mothers orally in groundnut oil six hours before sacrifice. The distribution of radioactivity of the two compounds was studied in maternal intestine, liver and plasma and fetal brain, heart liver lung and placenta. The transfer of /sup 3/H-retinoic acid across placenta was restricted as compared to that of /sup 3/H-retinyl acetate which may explain the reason why retinoic acid does not support fetal growth.

  9. Structural characterization of two tetra-chlorido-zincate salts of 4-carb-oxy-1H-imidazol-3-ium: a salt hydrate and a co-crystal salt hydrate.

    Science.gov (United States)

    Martens, Sean J; Geiger, David K

    2017-02-01

    Imidazole-containing compounds exhibit a myriad of pharmacological activities. Two tetra-chlorido-zincate salts of 4-carb-oxy-1H-imidazol-3-ium, ImHCO2H(+), are reported. Bis(4-carb-oxy-1H-imidazol-3-ium) tetra-chlorido-zincate monohydrate, (C4H5N2O2)2[ZnCl4]·H2O, (I), crystallizes as a monohydrate salt, while bis-(4-carb-oxy-1H-imidazol-3-ium) tetra-chlorido-zincate bis-(1H-imidazol-3-ium-4-carboxyl-ato) monohydrate, (C4H5N2O2)2[ZnCl4]·2C4H4N2O2·H2O, (II), is a co-crystal salt with six residues: two ImHCO2H(+) cations, two formula units of the zwitterionic 1H-imidazol-3-ium-4-carboxyl-ate, ImHCO2, one tetra-chlorido-zincate anion and one water mol-ecule disordered over two sites in a 0.60 (4):0.40 (4) ratio. The geometric parameters of the ImHCO2H(+) and the ImHCO2 moieties are the same within the standard uncertainties of the measurements. Both compounds exhibit extensive hydrogen bonding, including involvement of the tetra-chlorido-zincate anion, resulting in inter-connected chains of anions joined by water mol-ecules.

  10. Light dependence of [3H]leucine incorporation in the oligotrophic North Pacific ocean.

    Science.gov (United States)

    Church, Matthew J; Ducklow, Hugh W; Karl, David M

    2004-07-01

    The influence of irradiance on bacterial incorporation of [(3)H]leucine was evaluated at Station ALOHA in the oligotrophic North Pacific subtropical gyre. Six experiments were conducted on three cruises to Station ALOHA to examine how [(3)H]leucine incorporation varied as a function of irradiance. Two experiments were also conducted to assess the photoautotrophic response to irradiance (based on photosynthetic uptake of [(14)C]bicarbonate) in both the upper and lower photic zones. Rates of [(3)H]leucine incorporation responded to irradiance in a photosynthesis-like manner, increasing sharply at low light and then saturating and sometimes declining with increasing light intensity. The influence of irradiance on bacterial growth was evaluated in both the well-lit (5 to 25 m) and dimly lit regions of the upper ocean (75 to 100 m) to determine whether the bacterial response to irradiance differed along the depth-dependent light gradient of the photic zone. [(3)H]leucine incorporation rates were analyzed with a photosynthesis-irradiance model for a quantitative description of the relationships between [(3)H]leucine incorporation and irradiance. Maximum rates of [(3)H]leucine incorporation in the upper photic zone increased 48 to 92% relative to those of dark-incubated samples, with [(3)H]leucine incorporation saturating at light intensities between 58 and 363 micromol of quanta m(-2) s(-1). Rates of [(3)H]leucine incorporation in the deep photic zone were photostimulated 53 to 114% and were susceptible to photoinhibition, with rates declining at light intensities of >100 micromol of quanta m(-2) s(-1). The results of these experiments revealed that sunlight directly influences bacterial growth in this open-ocean ecosystem.

  11. Efficient synthesis of 4(3H)-quinazolinones using a soluble polymeric support

    Institute of Scientific and Technical Information of China (English)

    Chang Xie; Hong Xia Li; Ming Guo Liu; Ming Wu Ding

    2008-01-01

    4(3H)-Quinazolinones have been synthesized from poly(ethylene glycol) (PEG) supported aza-Wittig reaction. 2-Dialkylamino-4(3H)-quinazolinones 6 were synthesized efficiently by reaction of secondary amine with PEG-supported carbodiimides 4, whichwere obtained from aza-Wittig reaction of PEG-supported iminophosphoranes 3 with isocyanates.?2008 Ming Wu Ding. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

  12. [Pharmacokinetic study of 3H-stiripentol in rats (author's transl)].

    Science.gov (United States)

    Pieri, F; Wegmann, R; Astoin, J

    1982-01-01

    The radioactive constituents of blood, urine, and bile specimens from Wistar Rats, following intravenous administration of 3H-stiripentol were analyzed, in parallel with samples of: liver, lung, kidneys, testis, heart, brain, cerebellum, and medulla. These investigations yielded the following results: 3H-Stiripentol was quantitatively and rapidly absorbed and metabolized by Wistar rats, due to intense metabolism in the liver. The cerebellum and medulla accumulated radioactivity, which was probably related to the pharmacological effects of this drug.

  13. Chemical integrity of ( sup 3 H)GABA used in binding studies

    Energy Technology Data Exchange (ETDEWEB)

    Balcar, V.J. (Univ. of Sydney, N.S.W. (Australia))

    1989-07-01

    A method which is claimed to be able to determine the proportion of true GABA within radiolabeled GABA used in binding studies was tested using (3H)GABA. The method was found to be unsuitable for {sup 3}H-labeled GABA and, furthermore, both theoretical considerations and the present experimental data indicated that it could also produce misleading results with ({sup 14}C)GABA.

  14. Collisional excitation of doubly and triply deuterated ammonia ND$_2$H and ND$_3$ by H$_2$

    CERN Document Server

    Daniel, F; Faure, A; Roueff, E; Gérin, M; Lis, D C; Hily-Blant, P; Bacmann, A; Wiesenfeld, L

    2016-01-01

    The availability of collisional rate coefficients is a prerequisite for an accurate interpretation of astrophysical observations, since the observed media often harbour densities where molecules are populated under non--LTE conditions. In the current study, we present calculations of rate coefficients suitable to describe the various spin isomers of multiply deuterated ammonia, namely the ND$_2$H and ND$_3$ isotopologues. These calculations are based on the most accurate NH$_3$--H$_2$ potential energy surface available, which has been modified to describe the geometrical changes induced by the nuclear substitutions. The dynamical calculations are performed within the close--coupling formalism and are carried out in order to provide rate coefficients up to a temperature of $T$ = 50K. For the various isotopologues/symmetries, we provide rate coefficients for the energy levels below $\\sim$ 100 cm$^{-1}$. Subsequently, these new rate coefficients are used in astrophysical models aimed at reproducing the NH$_2$D, ...

  15. 5-[1-(1,3-Dimethyl-2,4,6-trioxohexahydropyrimidin-5-yl-2-oxopropyl]-1,3-dimethylpyrimidine-2,4,6(1H,3H,5H-trione

    Directory of Open Access Journals (Sweden)

    Manfred Steimann

    2013-08-01

    Full Text Available The title compound, C15H18N4O7, is a product of the substitution reaction of 5,5-dibromo-1,3-dimethylbarbituric acid with sodium sulfide in aqueous acetone. In the crystal, molecules display neither intermolecular nor intramolecular hydrogen bonding and the two barbiturate rings adopt the keto form.

  16. 3-{[3-(4-Methoxyphenyl-4,5-dihydro-1,2-oxazol-5-yl]methyl}-1,5-dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H-dione

    Directory of Open Access Journals (Sweden)

    Rachida Dardouri

    2011-07-01

    Full Text Available The molecule of the title compound, C22H23N3O4, features a benzodiazepine fused-ring system whose seven-membered ring adopts a boat-shaped conformation (with the C atoms of the fused-ring as the stern and the methine C atom as the prow. The methylene C atom connected to the methine C atom occupies an equatorial position. The methylene C atom is connected to the five-membered oxazole ring, both of which are disordered over two positions in a 0.634 (4:0.366 (4 ratio. Weak intermolecular C—H...O hydrogen bonding is present in the crystal structure.

  17. 6-Hydroxy-5-[(2-hydroxy-4,4-dimethyl-6-oxocyclohex-1-enyl(4-nitrophenylmethyl]-1,3-dimethylpyrimidine-2,4(1H,3H-dione

    Directory of Open Access Journals (Sweden)

    N. Sureshbabu

    2013-11-01

    Full Text Available In the title compound, C21H23N3O7, the pyrimidinedione ring adopts a screw-boat conformation, whereas the cyclohexenone ring adopts an envelope conformation, with the C atom bearing the methyl groups as the flap atom. The dihedral angle between the mean planes of the pyrimidinedione and cyclohexenone rings is 58.78 (2°. The pyrimidinedione and cyclohexenone rings form dihedral angles of 59.94 (3 and 54.73 (2°, respectively, with the 4-nitrophenyl ring. Relatively strong intramolecular O—H...O hydrogen bonds are observed. In the crystal, molecules are linked by C—H...O hydrogen bonds, forming a chain along the c-axis direction.

  18. Quantum chemical investigation of the intra- and intermolecular proton transfer reactions and hydrogen bonding interactions in 4-amino-5-(2-hydroxyphenyl)-2H-1,2,4-triazole-3(4H)-thione.

    Science.gov (United States)

    Özdemir, Namık

    2013-01-01

    The intramolecular thione-thiol tautomerism and intermolecular double proton transfer reaction of the hydrogen-bonded thione and thiol dimers in the title triazole compound were studied at the B3LYP level of theory using 6-311++G(d,p) basis function. The influence of the solvent on the single and double proton transfer reactions was examined in three solvents (chloroform, methanol and water) using the polarizable continuum model (PCM) approximation. The computational results show that the thione tautomer is the most stable isomer with a very high tautomeric energy barrier both in the gas phase and in solution phase, indicating a quite disfavored process. The solvent effect is found to be sizable with increasing polarity. In the double proton transfer reaction, the thione dimer is found to be more stable than thiol dimer both in the gas phase and in solution phase. The energetic and thermodynamic parameters of the double proton transfer process show that the double proton exchange from thione dimer to thiol dimer is thermodynamically unfavored. However, the exchange from thiol dimer to thione dimer for the gas phase and water phase seems to be feasible with a low barrier height and with a negative value in enthalpy and free energy changes. In addition, the hydrogen bonding interactions were analyzed in the gas phase regarding their geometries and energies. It is found that all complex formations are enthalpically favored, and the stability of the H-bonds comes in the order of S1-H2···N2>N2-H2···S1>N3-H3B···O1. Finally, non-linear optical properties were carried out at the same calculation level in the gas phase.

  19. 2H NMR studies of glycerol dynamics in protein matrices.

    Science.gov (United States)

    Herbers, C R; Sauer, D; Vogel, M

    2012-03-28

    We use (2)H NMR spectroscopy to investigate the rotational motion of glycerol molecules in matrices provided by the connective tissue proteins elastin and collagen. Analyzing spin-lattice relaxation, line-shape properties, and stimulated-echo decays, we determine the rates and geometries of the motion as a function of temperature and composition. It is found that embedding glycerol in an elastin matrix leads to a mild slowdown of glycerol reorientation at low temperatures and glycerol concentrations, while the effect vanishes at ambient temperatures or high solvent content. Furthermore, it is observed that the nonexponential character of the rotational correlation functions is much more prominent in the elastin matrix than in the bulk liquid. Results from spin-lattice relaxation and line shape measurements indicate that, in the mixed systems, the strong nonexponentiality is in large part due to the existence of distributions of correlation times, which are broader on the long-time flank and, hence, more symmetric than in the neat system. Stimulated-echo analysis of slow glycerol dynamics reveals that, when elastin is added, the mechanism for the reorientation crosses over from small-angle jump dynamics to large-angle jump dynamics and the geometry of the motion changes from isotropic to anisotropic. The results are discussed against the background of present and previous findings for glycerol and water dynamics in various protein matrices and compared with observations for other dynamically highly asymmetric mixtures so as to ascertain in which way the viscous freezing of a fast component in the matrix of a slow component differs from the glassy slowdown in neat supercooled liquids.

  20. High/variable mixture ratio O2/H2 engine

    Science.gov (United States)

    Adams, A.; Parsley, R. C.

    1988-01-01

    Vehicle/engine analysis studies have identified the High/Dual Mixture Ratio O2/H2 Engine cycle as a leading candidate for an advanced Single Stage to Orbit (SSTO) propulsion system. This cycle is designed to allow operation at a higher than normal O/F ratio of 12 during liftoff and then transition to a more optimum O/F ratio of 6 at altitude. While operation at high mixture ratios lowers specific impulse, the resultant high propellant bulk density and high power density combine to minimize the influence of atmospheric drag and low altitude gravitational forces. Transition to a lower mixture ratio at altitude then provides improved specific impulse relative to a single mixture ratio engine that must select a mixture ratio that is balanced for both low and high altitude operation. This combination of increased altitude specific impulse and high propellant bulk density more than offsets the compromised low altitude performance and results in an overall mission benefit. Two areas of technical concern relative to the execution of this dual mixture ratio cycle concept are addressed. First, actions required to transition from high to low mixture ratio are examined, including an assessment of the main chamber environment as the main chamber mixture ratio passes through stoichiometric. Secondly, two approaches to meet a requirement for high turbine power at high mixture ratio condition are examined. One approach uses high turbine temperature to produce the power and requires cooled turbines. The other approach incorporates an oxidizer-rich preburner to increase turbine work capability via increased turbine mass flow.

  1. 2H NMR studies of glycerol dynamics in protein matrices

    Science.gov (United States)

    Herbers, C. R.; Sauer, D.; Vogel, M.

    2012-03-01

    We use 2H NMR spectroscopy to investigate the rotational motion of glycerol molecules in matrices provided by the connective tissue proteins elastin and collagen. Analyzing spin-lattice relaxation, line-shape properties, and stimulated-echo decays, we determine the rates and geometries of the motion as a function of temperature and composition. It is found that embedding glycerol in an elastin matrix leads to a mild slowdown of glycerol reorientation at low temperatures and glycerol concentrations, while the effect vanishes at ambient temperatures or high solvent content. Furthermore, it is observed that the nonexponential character of the rotational correlation functions is much more prominent in the elastin matrix than in the bulk liquid. Results from spin-lattice relaxation and line shape measurements indicate that, in the mixed systems, the strong nonexponentiality is in large part due to the existence of distributions of correlation times, which are broader on the long-time flank and, hence, more symmetric than in the neat system. Stimulated-echo analysis of slow glycerol dynamics reveals that, when elastin is added, the mechanism for the reorientation crosses over from small-angle jump dynamics to large-angle jump dynamics and the geometry of the motion changes from isotropic to anisotropic. The results are discussed against the background of present and previous findings for glycerol and water dynamics in various protein matrices and compared with observations for other dynamically highly asymmetric mixtures so as to ascertain in which way the viscous freezing of a fast component in the matrix of a slow component differs from the glassy slowdown in neat supercooled liquids.

  2. Effect of SO2 on the performance of Ag-Pd/Al2O3 for the selective catalytic reduction of NOx with C2H5OH

    Institute of Scientific and Technical Information of China (English)

    XIE Shu-xia; YU Yun-bo; WANG Jin; HE Hong

    2006-01-01

    The influence of SO2 on the performance of Ag-Pd/Al2O3 for the selective catalytic reduction (SCR) of NOx with C2H5OH was investigated experimentally. The activity test results suggest that Ag-Pd/Al2O3 shows a small activity loss in the presence of SO2 when using C2H5OH as a reductant. In situ DRIFTS spectra show that the activity loss originates from the formation of surface sulphate species on the Ag-Pd/Al2O3. The surface sulphate species formation inhibits the formation of nitrate, whereas hardly changes the partial oxidation of C2H5OH. Compared with the NOx reduction by C3H6, an obvious suppression of the surface sulphate species formation was observed by DRIFTS experiment when using C2H5OH as a reductant. This phenomenon reveals the better catalytic performance and strong SO2 tolerance of Ag-Pd/Al2O3-C2H5OH system.

  3. High-affinity binding of (/sup 3/H)acetylcholine to muscarinic cholinergic receptors

    Energy Technology Data Exchange (ETDEWEB)

    Kellar, K.J.; Martino, A.M.; Hall, D.P. Jr.; Schwartz, R.D.; Taylor, R.L.

    1985-06-01

    High-affinity binding of (/sup 3/H)acetylcholine to muscarinic cholinergic sites in rat CNS and peripheral tissues was measured in the presence of cytisin, which occupies nicotinic cholinergic receptors. The muscarinic sites were characterized with regard to binding kinetics, pharmacology, anatomical distribution, and regulation by guanyl nucleotides. These binding sites have characteristics of high-affinity muscarinic cholinergic receptors with a Kd of approximately 30 nM. Most of the muscarinic agonist and antagonist drugs tested have high affinity for the (/sup 3/H)acetylcholine binding site, but pirenzepine, an antagonist which is selective for M-1 receptors, has relatively low affinity. The ratio of high-affinity (/sup 3/H)acetylcholine binding sites to total muscarinic binding sites labeled by (/sup 3/H)quinuclidinyl benzilate varies from 9 to 90% in different tissues, with the highest ratios in the pons, medulla, and heart atrium. In the presence of guanyl nucleotides, (/sup 3/H) acetylcholine binding is decreased, but the extent of decrease varies from 40 to 90% in different tissues, with the largest decreases being found in the pons, medulla, cerebellum, and heart atrium. The results indicate that (/sup 3/H)acetylcholine binds to high-affinity M-1 and M-2 muscarinic receptors, and they suggest that most M-2 sites have high affinity for acetylcholine but that only a small fraction of M-1 sites have such high affinity.

  4. Dopamine D2 receptor radiotracers [{sup 11}C](+)-PHNO and [{sup 3}H]raclopride are indistinguishably inhibited by D2 agonists and antagonists ex vivo

    Energy Technology Data Exchange (ETDEWEB)

    McCormick, Patrick N. [Institute of Medical Science, University of Toronto, Toronto, Ontario, M5S 1A8 (Canada)], E-mail: patrick.mccormick@camhpet.ca; Kapur, Shitij [Department of Psychiatry, University of Toronto, Toronto, Ontario, M5S 1A8 (Canada); PET Center, Center for Addiction and Mental Health, Toronto, Ontario, M5T 1R8 (Canada); Seeman, Philip [Department of Psychiatry, University of Toronto, Toronto, Ontario, M5S 1A8 (Canada); Department of Pharmacology, University of Toronto, Toronto, Ontario, M5S 1A8 (Canada); Wilson, Alan A. [Department of Psychiatry, University of Toronto, Toronto, Ontario, M5S 1A8 (Canada); PET Center, Center for Addiction and Mental Health, Toronto, Ontario, M5T 1R8 (Canada)

    2008-01-15

    Introduction: In vitro, the dopamine D2 receptor exists in two states, with high and low affinity for agonists. The high-affinity state is the physiologically active state thought to be involved in dopaminergic illnesses such as schizophrenia. The positron emission tomography radiotracer [{sup 11}C](+)-PHNO ([{sup 11}C](+)-4-propyl-3,4,4a,5,6,10b-hexahydro-2H-naphtho[1,2-b][1,4] oxazin-9-o l), being a D2 agonist, should selectively label the high-affinity state at tracer dose and therefore be more susceptible to competition by agonist as compared to the antagonist [{sup 3}H]raclopride, which binds to both affinity states. Methods: We tested this prediction using ex vivo dual-radiotracer experiments in conscious rats. D2 antagonists (haloperidol or clozapine), a partial agonist (aripiprazole), a full agonist [(-)-NPA] or the dopamine-releasing drug amphetamine (AMPH) were administered to rats prior to an intravenous coinjection of [{sup 11}C](+)-PHNO and [{sup 3}H]raclopride. Rats were sacrificed 60 min after radiotracer injection. Striatum, cerebellum and plasma samples were counted for {sup 11}C and {sup 3}H. The specific binding ratio {l_brace}SBR, i.e., [%ID/g (striatum)-%ID/g (cerebellum)]/(%ID/g (cerebellum){r_brace} was used as the outcome measure. Results: In response to D2 antagonists, partial agonist or full agonist, [{sup 11}C](+)-PHNO and [{sup 3}H]raclopride SBRs responded indistinguishably in terms of both ED{sub 50} and Hill slope (e.g., (-)-NPA ED{sub 50} values are 0.027 and 0.023 mg/kg for [{sup 11}C](+)-PHNO and [{sup 3}H]raclopride, respectively). In response to AMPH challenge, [{sup 11}C](+)-PHNO and [{sup 3}H]raclopride SBRs were inhibited to the same degree. Conclusions: We have shown that the SBRs of [{sup 11}C](+)-PHNO- and [{sup 3}H]raclopride do not differ in their response to agonist challenge. These results do not support predictions of the in vivo binding behavior of a D2 agonist radiotracer and cast some doubt on the in vivo

  5. The structure of Fe sub 2 (PO sub 3 H) sub 3. Structure du phosphite de Fer: Fe sub 2 (PO sub 3 H) sub 3

    Energy Technology Data Exchange (ETDEWEB)

    Sghyar, M. (Lab. de Chimie Minerale Appliquee, Faculte des Sciences, Fes (Morocco)); Durand, J.; Cot, L. (Lab. de Physicochimie des Materiaux, Ecole Nationale Superieure de Chimie de Montpellier, 34 - Motpellier (France)); Rafiq, M. (Lab. de Chimie Minerale Appliquee, Faculte des Sciences, Fes (Morocco))

    1992-12-15

    M{sub r}=351.7, hexagonal, P6{sub 3}/m, a=8.037(2), c=7.352(2) A, V=411.3(3) A{sup 3}, Z=4, D{sub m}=5.664 (by pycnometry), D{sub x}=5.682 Mg m{sup -3}, {lambda}(Mo K{alpha})=0.71069 A, {mu}=39.79 mm{sup -1}, F(000)=292, room temperature, final R=0.028, wR=0.035 for 397 independent reflections. Fe{sub 2}(PO{sub 3}H){sub 3} has been studied by single-crystal X-ray analysis with an automatic diffractometer. The structure is built from one pair of face-sharing octahedra perpendicular to the c axis. PO{sub 3}H{sup 2-} tetrahedra and FeO{sub 6} octahedra only share vertices. Hydrogen atoms of the PO{sub 3}H{sup 2-} anions are in the 3 A diameter channel around the 6{sub 3} axis. (orig.).

  6. Measurement of extremely (2) H-enriched water samples by laser spectrometry: application to batch electrolytic concentration of environmental tritium samples.

    Science.gov (United States)

    Wassenaar, L I; Kumar, B; Douence, C; Belachew, D L; Aggarwal, P K

    2016-02-15

    Natural water samples artificially or experimentally enriched in deuterium ((2) H) at concentrations up to 10,000 ppm are required for various medical, environmental and hydrological tracer applications, but are difficult to measure using conventional stable isotope ratio mass spectrometry. Here we demonstrate that off-axis integrated cavity output (OA-ICOS) laser spectrometry, along with (2) H-enriched laboratory calibration standards and appropriate analysis templates, allows for low-cost, fast, and accurate determinations of water samples having δ(2) HVSMOW-SLAP values up to at least 57,000 ‰ (~9000 ppm) at a processing rate of 60 samples per day. As one practical application, extremely (2) H-enriched samples were measured by laser spectrometry and compared to the traditional (3) H Spike-Proxy method in order to determine tritium enrichment factors in the batch electrolysis of environmental waters. Highly (2) H-enriched samples were taken from different sets of electrolytically concentrated standards and low-level (tritium samples, and all cases returned accurate and precise initial low-level (3) H results. The ability to quickly and accurately measure extremely (2) H-enriched waters by laser spectrometry will facilitate the use of deuterium as a tracer in numerous environmental and other applications. For low-level tritium operations, this new analytical ability facilitated a 10-20 % increase in sample productivity through the elimination of spike standards and gravimetrics, and provides immediate feedback on electrolytic enrichment cell performance. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  7. Full-dimensional quantum dynamics study of the H2 + C2H → H + C2H2 reaction on an ab initio potential energy surface

    Science.gov (United States)

    Chen, Liuyang; Shao, Kejie; Chen, Jun; Yang, Minghui; Zhang, Dong H.

    2016-05-01

    This work performs a time-dependent wavepacket study of the H2 + C2H → H + C2H2 reaction on a new ab initio potential energy surface (PES). The PES is constructed using neural network method based on 68 478 geometries with energies calculated at UCCSD(T)-F12a/aug-cc-pVTZ level and covers H2 + C2H↔H + C2H2, H + C2H2 → HCCH2, and HCCH2 radial isomerization reaction regions. The reaction dynamics of H2 + C2H → H + C2H2 are investigated using full-dimensional quantum dynamics method. The initial-state selected reaction probabilities are calculated for reactants in eight vibrational states. The calculated results showed that the H2 vibrational excitation predominantly enhances the reactivity while the excitation of bending mode of C2H slightly inhibits the reaction. The excitations of two stretching modes of C2H molecule have negligible effect on the reactivity. The integral cross section is calculated with J-shift approximation and the mode selectivity in this reaction is discussed. The rate constants over 200-2000 K are calculated and agree well with the experimental measured values.

  8. Metabolism of (/sup 3/H)noradrenaline in different compartments of rat brain with respect to the role of catechol-O-methyltransferase

    Energy Technology Data Exchange (ETDEWEB)

    Koester, G.; Goede, E.; Breuer, H.

    1984-03-01

    Rats were pretreated with either reserpine or desmethylimipramine, either alone or in combination with tropolone. At either 10 min or 1 h after the intraventricular injection of (/sup 3/H)noradrenaline, in several brain regions the complete metabolic patterns were determined: normetanephrine; the glycol metabolites (methylated and nonmethylated) and their sulfate conjugates; and the acidic metabolites (methylated and non-methylated). A reserpine-induced increase in the turnover of (/sup 3/H)noradrenaline caused a transient increase of the catechol glycol followed by elevated levels of the two glycol sulfates. The stimulated (/sup 3/H)noradrenaline turnover if achieved by desmethylimipramine caused a transient increase of normetanephrine and initially lowered values of catechol glycols (both free and sulfated), which were followed by elevated levels. Drug-pretreated rats compensated for the inhibition of catechol-O-methyl-transferase by tropolone in different ways: Reserpine caused an early increase of the catechol glycol beyond the measurements in other treatment groups, whereas desmethylimipramine increased the nonmethylated carboxylic acid and glycol sulfates rather slowly to levels beyond those of other groups. The results support the existence of two compartments with a fast metabolism (an intraneuronal monoamine oxidase compartment and an extraneuronal catechol-O-methyltransferase compartment). In addition, there seems to exist another extra-neuronal space with a slow, monoamine oxidase-dependent noradrenaline turnover.

  9. Structure, DNA Binding Studies and Cytotoxicity of Complex [Pd(phen)(L-asp)]·3H2O

    Institute of Scientific and Technical Information of China (English)

    GAO Enjun; LIU Lei; SHI Chunyue; YIN Hongxi; ZHU Mingchang; WU Qiong; LIU Qitao

    2009-01-01

    The pal ladium(Ⅱ) complex of [Pd(phen)(L-asp)].3H2O (phen= 1,10-phenanthroline, H2L-asp=L-aspartic acid) has been synthesized from a solution reaction and analyzed by elemental analyses, 1H NMR and IR spectra. More-over, the complex has been structurally characterized by single-crystal X-ray diffractometry. The cytotoxicity assay of the complex and cis-DDP as reference substance against three different cancer cell lines (Hela, Hep-G2 and KB)has been conducted. The results show that the Pd complex exhibits higher cytotoxicity against Hela system. The study on the interaction of the Pd complex with fish sperm DNA (FS-DNA) has been performed with diverse spec-troscopic techniques, showing that the complex is bound to the fish sperm DNA via an intercalative mode. Gel elec-trophoresis assay demonstrates the ability of the complex to cleave the pBR 322 plasmid DNA.

  10. A comparison of 2H2O and phenylalanine flooding dose to investigate muscle protein synthesis with acute exercise in rats

    Science.gov (United States)

    Gasier, Heath G.; Riechman, Steven E.; Wiggs, Michael P.; Previs, Stephen F.; Fluckey, James D.

    2009-01-01

    The primary objective of this investigation was to determine whether 2H2O and phenylalanine (Phe) flooding dose methods yield comparable fractional rates of protein synthesis (FSR) in skeletal muscle following a single bout of high-intensity resistance exercise (RE). Sprague-Dawley rats were assigned by body mass to either 4-h control (CON 4 h; n = 6), 4-h resistance exercise (RE 4 h; n = 6), 24-h control (CON 24 h; n = 6), or 24-h resistance exercise (RE 24 h; n = 6). The RE groups were operantly conditioned to engage in a single bout of high-intensity, “squat-like” RE. All rats were given an intraperitoneal injection of 99.9% 2H2O and provided 4.0% 2H2O drinking water for either 24 (n = 12) or 4 h (n = 12) prior to receiving a flooding dose of l-[2,3,4,5,6-3H]Phe 16 h post-RE. Neither method detected an effect of RE on FSR in the mixed gastrocnemius, plantaris, or soleus muscle. Aside from the qualitative similarities between methods, the 4-h 2H2O FSR measurements, when expressed in percent per hour, were quantitatively greater than the 24-h 2H2O and Phe flooding in all muscles (P < 0.001), and the 24-h 2H2O was greater than the Phe flooding dose in the mixed gastrocnemius and plantaris (P < 0.05). In contrast, the actual percentage of newly synthesized protein was significantly higher in the 24- vs. 4-h 2H2O and Phe flooding dose groups (P < 0.001). These results suggest that the methodologies provide “qualitatively” similar results when a perturbation such as RE is studied. However, due to potential quantitative differences between methods, the experimental question should determine what approach should be used. PMID:19366878

  11. Synthesis and Characterization of Novel 1H-Indazole Derivatives%1H-吲唑类中间体的合成及表征

    Institute of Scientific and Technical Information of China (English)

    周淑晶; 李长胜; 关文碧; 武晓丽; 刘雪; 马永强

    2013-01-01

    以取代邻甲苯胺为原料经乙酰化、溴化、环合及胺解反应得到1H-吲唑类化合物,再与酸酐、碘乙烷或硝酸反应以较高收率合成了15个1H-吲唑衍生物,其中12个未见文献报道.其结构经1H NMR、IR表征确认.

  12. 无催化剂条件下的全氟烷基取代的1H-苯并[b][1,4]二氮(革)-2(3H)-酮的简易合成%Facile Synthesis of Perfluoroalkyl Substituted 1H-Benzo[b][1,4]-diazepine-2(3H)-ones via a Catalyst-Free Process

    Institute of Scientific and Technical Information of China (English)

    翟士燕; 曹卫国; 张慧

    2013-01-01

    1,5-苯并二氮(革)-2-酮作为一个独特的骨架广泛存在于很多具有生理活性的化合物中,而全氟烷基的引入影响到有机化合物的理化性质以及生理活性的改变.因此将全氟代烷基引入1,5-苯并二氮(革)-2-酮的方法的研究正变得日趋重要.发展了一个制备全氟代烷基取代的1,5-苯并二氮(革)-2-酮的简易方法.采用全氟代炔酸甲酯为含氟砌块,与邻芳基二胺,以无水甲苯为溶剂,在无催化剂存在条件下,80℃反应24 h,以较好的收率顺利得到4-全氟烷基-1,3-二氢-1,5-苯并二氮(革)-2-酮类化合物.%l,5-Benzodiazepin-2-one is a privileged scaffold and compounds containing such substructures exhibit a range of biological activities. Perfluoroalkyl groups can favorably affect the physical and biological properties of organic compounds. Accordingly, the development of methods to introduce perfluoroalkyl groups into 1,5-benzodiazepin-2-ones has become increasingly important. Herein, an efficient and simple route for preparation of perfluoroalkylated l,5-benzodiazepine-2-ones is described. The reaction of methyl 3-perfluoroalkyl-2-alkynoate as the fluorinated building block with o-arylenediamine proceeds smoothly in dry toluene at 80 ℃ for 24 h without any catalyst to afford the titled compounds in good yields.

  13. Synthesis, Characterization and Crystal Structure of Some Novel 1-(3,5-Dimethyl-1 H-pyrazol-l-yl)-3-(substituted anilino)propan-l-ones

    Institute of Scientific and Technical Information of China (English)

    SAEED Aamer; HUSSAIN Shahid; ABBAS Naeem; BOLTE Michael

    2009-01-01

    Michael addition of some substituted anilines to methyl acrylate in acidic medium afforded the methyl 3-(substituted anilino)propionates (1a-1i), which on treatment with hydrazine hydrate in methanol were converted into corresponding 3-(substituted anilino) propionohydrazides (2a-2i) in good yields. Microwave irradiation of the latter with pentane-2,4-dione afforded 1-(3,5-dimethyl- 1H-pyrazol-1-y1)-3-(substituted anilino)propan- 1-ones (3a-3i) under solventless conditions. The structures were confirmed by spectroscopic data, elemental analyses and in case of the 3h by single crystal X-ray diffraction data.

  14. Characterization and regulation of (/sup 3/H)-serotonin uptake and release in rodent spinal

    Energy Technology Data Exchange (ETDEWEB)

    Stauderman, K.A.

    1986-01-01

    The uptake and release of (/sup 3/H)-serotonin were investigated in rat spinal cord synaptosomes. In the uptake experiments, sodium-dependent and sodium-independent (/sup 3/H)-serotonin accumulation processes were found. Sodium-dependent (/sup 3/H)-serotonin accumulation was: linear with sodium concentrations up to 180 mM; decreased by disruption of membrane integrity or ionic gradients; associated with purified synaptosomal fractions; and reduced after description of descending serotonergic neurons in the spinal cord. Of the uptake inhibitors tested, the most potent was fluoxetine (IC/sub 50/ 75 nM), followed by desipramine (IC/sub 50/ 430 nM) and nomifensine (IC/sub 50/ 950 nM). The sodium-independent (/sup 3/H)-serotonin accumulation process was insensitive to most treatments and probably represents nonspecific membrane binding. Thus, only sodium-dependent (/sup 3/H)-serotonin uptake represents the uptake process of serotonergic nerve terminals in rat spinal cord homogenates. In the release experiments, K/sup +/-induced release of previously accumulated (/sup 3/H)-serotonin was Ca/sup 2 +/-dependent, and originated from serotonergic synaptosomes. Exogenous serotonin and 5-methyoxy-N,N-dimethyltryptamine inhibited (/sup 3/H)-serotonin release in a concentration-dependent way. Of the antagonists tested, only methiothepin effectively blocked the effect of serotonin. These data support the existence of presynaptic serotonin autoreceptors on serotonergic nerve terminals in the rat spinal cord that act to inhibit a voltage and Ca/sup 2 +/-sensitive process linked to serotonin release. Alteration of spinai cord serotonergic function may therefore be possible by drugs acting on presynaptic serotonin autoreceptors in the spinal cord.

  15. Depletion of (/sup 3/H)methyltrienolone cytosol binding in glucocorticoid-induced muscle atrophy (42001)

    Energy Technology Data Exchange (ETDEWEB)

    Kurowski, T.T.; Capaccio, J.A.; Chatterton, R.T. Jr.; Hickson, R.C.

    1985-01-01

    The present study was undertaken to determine cytosol binding properties of (/sup 3/H)methyltrienolone, a synthetic androgen, in comparison with (/sup 3/)dexamethasone, a synthetic glucocorticoid, under conditions of glucocorticoid excess in skeletal muscle. Male hypophysectomized rats received either seven daily subcutaneous injections of cortisone acetate (CA) (100 mg x kg/sup -1/ body wt) or the vehicle, 1% carboxymethyl cellulose. Following treatment, both (/sup 3/H)dexamethansone and (/sup 3/H)methyltrienolone-receptor concentrations were decreased from those in vehicle-treated rats by more than 90 and 80%, respectively, in CA-treated animals. Scatchard analysis of (/sup 3/H)methyltrienolone binding in muscles of vehicle-treated animals became nonlinear at high concentrations of labeled ligand and were reanalyzed by a two-component binding model. The lower affinity, higher capacity component, which was attributed to binding of methyltrienolone to a dexamethasone component, which was attributed to binding of methyltrienolone to a dexamethasone component, disappeared in muscles of CA-treated rats and Scatchard plots were linear. Receptor concentrations of the higher affinity lower capacity methyltrienolone component were similar in muscles of vehicle-treated and CA-treated groups. From competition studies, the high relative specificities of glucocorticoids for (/sup 3/H)methyltrienolone binding in muscles of vehicle-treated animals were markedly reduced by CA treatment. In addition, the binding specificity data also showed strong competition by progesterone and methyltrienolone for (/sup 3/H)dexamethasone binding and estradiol-17..beta.. for (/sup 3/H)methyltrienolone binding.

  16. Characterizing a sewage plume using the 3H-3He dating technique

    Science.gov (United States)

    Shapiro, Stephanie Dunkle; LeBlanc, Denis; Schlosser, Peter; Ludin, Andrea

    1999-01-01

    An extensive 3H-3He study was performed to determine detailed characteristics of a regional flow system and a sewage plume over a distance of 4 km in a sand and gravel aquifer at Otis Air Base in Falmouth, Massachusetts. 3H-3He ages increase with depth in individual piezometer clusters and with distance along flowpaths. However, the age gradient with depth (Δt/Δz) is smaller in the plume than that in the regional waters, due to the intense recharge in the infiltration beds. The 1960s bomb peak of tritium in precipitation is archived longitudinally along a flowline through the main axis of the plume and vertically in individual piezometer clusters. On the eastern side of the sampling area, where water from Ashumet Pond forces plume water deeper into the flow system, 3H-3He ages are young at depth because the 3H-3He "clock" is reset due to outgassing of helium in the pond. A reconstruction of the tritium input functions for the regional and plume samples shows that there is no offset in the peak [3H]+[3Hetrit] concentrations for the plume and regional water, indicating that the water from supply wells for use on the base is young. The 3H-3He ages and detergent concentrations in individual wells are consistent with the beginning of use of detergents and the time period when their concentrations in sewage would have been greatest. Ages and hydraulic properties calculated using the 3H-3He data compare well with those from previous investigations and from particle-tracking simulations.

  17. Characterization of (/sup 3/H)paroxetine binding in rat brain

    Energy Technology Data Exchange (ETDEWEB)

    Marcusson, J.O.; Bergstroem, M.E.; Eriksson, K.; Ross, S.B.

    1988-06-01

    The binding of the 5-hydroxytryptamine (5-HT, serotonin) uptake inhibitor (3H)paroxetine to rat cortical homogenates has been characterized. The effect of tissue concentration was examined and, with 0.75 mg wet weight tissue/ml in a total volume of 1,600 microliter, the binding was optimized with an apparent dissociation constant (KD) of 0.03-0.05 nM. Competition experiments with 5-HT, citalopram, norzimeldine, and desipramine revealed a high (90%) proportion of displaceable binding that fitted a single-site binding model. Fluoxetine and imipramine revealed, in addition to a high-affinity (nanomolar) site, also a low-affinity (micromolar) site representing approximately 10% of the displaceable binding. The specificity of the (3H)paroxetine binding was emphasized by the fact that 5-HT was the only active neurotransmitter bound and that the serotonin S1 and S2 antagonist methysergide was without effect on the binding. Both 5-HT- and fluoxetine-sensitive (3H)paroxetine binding was completely abolished after protease treatment, suggesting that the binding site is of protein nature. Saturation studies with 5-HT (100 microM) sensitive (3H)paroxetine binding were also consistent with a single-site binding model, and the binding was competitively inhibited by 5-HT and imipramine. The number of binding sites (Bmax) for 5-HT-sensitive (3H)paroxetine and (3H)imipramine binding was the same, indicating that the radioligands bind to the same sites. Lesion experiments with p-chloroamphetamine resulted in a binding in frontal and parietal cortices becoming undetectable and a greater than 60% reduction in the striatum and hypothalamus, indicating a selective localization on 5-HT terminals. Together these findings suggest that (3H)paroxetine specifically and selectively labels the substrate recognition site for 5-HT uptake in rat brain.

  18. Ascorbic acid enables reversible dopamine receptor /sup 3/H-agonist binding

    Energy Technology Data Exchange (ETDEWEB)

    Leff, S.; Sibley, D.R.; Hamblin, M.; Creese, I.

    1981-11-16

    The effects of ascorbic acid on dopaminergic /sup 3/H-agonist receptor binding were studied in membrane homogenates of bovine anterior pituitary and caudate, and rat striatum. In all tissues virtually no stereospecific binding (defined using 1uM (+)butaclamol) of the /sup 3/H-agonists N-propylnorapomorphine (NPA), apomorphine, or dopamine could be demonstrated in the absence of ascorbic acid. Although levels of total /sup 3/H-agonist binding were three to five times greater in the absence than in the presence of 0.1% ascorbic acid, the increased binding was entirely non-stereospecific. Greater amounts of dopamine-inhibitable /sup 3/H-NPA binding could be demonstrated in the absence of 0.1% ascorbic acid, but this measure of ''specific binding'' was demonstrated not to represent dopamine receptor binding since several other catecholamines and catechol were equipotent with dopamine and more potent than the dopamine agonist (+/-)amino-6,7-dihydroxy-1,2,3,4-tetrahydronapthalene (ADTN) in inhibiting this binding. High levels of dopamine-displaceable /sup 3/H-agonist binding were detected in fresh and boiled homogenates of cerebellum, an area of brain which receives no dopaminergic innervation, further demonstrating the non-specific nature of /sup 3/H-agonist binding in the absence of ascorbic acid. These studies emphasize that under typical assay conditions ascorbic acid is required in order to demonstrate reversible and specific /sup 3/H-agonist binding to dopamine receptors.

  19. Photodegradation of amoxicillin by catalyzed Fe3+/H2O2 process

    Institute of Scientific and Technical Information of China (English)

    Xiaoming Li; Tingting Shen; Dongbo Wang; Xiu Yue; Xian Liu; Qi Yang; Jianbin Cao; Wei Zheng; Guangming Zeng

    2012-01-01

    Three oxidation processes of UV-Fe3+(EDTA)/H2O2 (UV:ultraviolet light; EDTA:ethylenediaminetetraacetic acid),UV-Fe3+/H2O2 and Fe3+/H2O2 were simultaneously investigated for the degradation of amoxicillin at pH 7.0.The results indicated that,100% amoxicillin degradation and 81.9% chemical oxygen demand (CODcr) removal could be achieved in the UV-Fe3+ (EDTA)/H2O2 process.The treatment efficiency of amoxicillin and CODcr removal were found to decrease to 59.0% and 43.0% in the UV-Fe3+/H2O2 process;39.6% and 31.3% in the Fe3+/H2O2 process.Moreover,the results of biodegradability (biological oxygen demand (BOD5)/CODCr ratio) revealed that the UV-Fe3+ (EDTA)/H2O2 process was a promising strategy to degrade amoxicillin as the biodegradability of the effluent was improved to 0.45,compared with the cases of UV-Fe3+/H2O2 (0.25) and Fe3+/H2O2 (0.10) processes.Therefore,it could be deduced that EDTA and UV light performed synergetic catalytic effect on the Fe3+/H2O2 process,enhancing the treatment efficiency.The degradation mechanisms were also investigated via UV-Vis spectra,and high performance liquid chromatography-mass spectra.The degradation pathway of amoxicillin was further proposed.

  20. Design and Synthesis of Some Thiazolidin-4-ones Based on (7-Hydroxy-2-oxo-2H-chromen-4-yl Acetic Acid

    Directory of Open Access Journals (Sweden)

    Valentina Rajkovic

    2009-07-01

    Full Text Available (7-Hydroxy-2-oxo-2H-chromen-4-yl-acetic acid methyl ester(1 upon reaction with ethyl bromoacetate furnishes (7-ethoxycarbonylmethoxy-2-oxo-2H-chromen-4-yl-acetic acid methylester (2, which on treatment with 100% hydrazine hydrate yields (7-hydrazinocarbonylmethoxy-2-oxo-2H-chromen-4-yl-acetic acid hydrazide (3. The condensation of compound 3 with different aromatic aldehydes afforded a series of [7-(arylidenehydrazinocarbonylmethoxy-2-oxo-2H-chromen-4-yl]-acetic acid arylidene-hydrazide Schiff’s bases 4a-k. Cyclo-condensation of compounds 4a-k with 2-mercapto-acetic acid in N,N-dimethylformamide in the presence of anhydrous ZnCl2 affordsN-(2-aryl-4-oxothiazolidin-3-yl-2-(4-(2-aryl-4-oxothiazolidin-3-ylcarbamoyl-methyl-2-oxo-2H-chromen-7-yloxy-acetamides 5a-k. Structure elucidation of the products has been accomplished on the basis of elemental analysis, IR, 1H-NMR and 13C-NMR data. Compounds 4a-k and 5a-k will be screened for their antibacterial activity against both Gram-positive and Gram-negative bacteria and the results reported elsewhere in due course.