Novel 2,3-Dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones: Synthesis and Biological Evaluation

Directory of Open Access Journals (Sweden)

Malose J. Mphahlele

2016-12-01

Full Text Available Herein we describe the synthesis and evaluation of a series of novel 2,3-dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones for in vitro cytotoxicity against three human cancer cell lines as well as for potential antimalarial activity against the chloroquine-sensitive strain 3D7 of Plasmodium falciparum. The title compounds were prepared via PdCl2-mediated endo-dig cyclization of 2-aryl-8-(arylethynyl-6-bromo-2,3-dihydroquinazolin-4(1H-ones. The latter were prepared, in turn, via initial Sonogashira cross-coupling of 2-amino-5-bromo-3-iodobenzamide with aryl acetylenes followed by boric acid-mediated cyclocondensation of the intermediate 2-amino-3-(arylethynyl-5-bromobenzamides with benzaldehyde derivatives. The 2,3-dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones 4a–k were evaluated for potential in vitro cytotoxicity against the breast (MCF-7, melanoma (B16 and endothelioma (sEnd.2 cell lines. All of the compounds except 4h and 4i were found to be inactive against the three cancer cell lines. Compound 4h substituted with a 4-methoxyphenyl and 4-fluorophenyl groups at the 3- and 5-positions was found to exhibit significant cytotoxicity against the three cancer cell lines. The presence of phenyl and 3-chlorophenyl groups at the 3- and 5-posiitons of the pyrroloquinazolinone 4i, on the other hand, resulted in significant cytotoxicity against vascular tumour endothelial cells (sEnd.2, but reduced activity against the melanoma (B16 and breast cancer (MCF-7 cells except at higher concentrations. The 2,3-dihydro-1H-pyrrolo[3,2,1-ij]quinazolin-1-ones 4a–l were found to be inactive against the chloroquine sensitive 3D7 strain of Plasmodium falciparum.

Ion radical rupture of the carbon-carbon bond in oxidation of 1,3,1',3'-tetramethyl-2,3,2',3'- tetrahydro-2,2'-diperimidinyl

International Nuclear Information System (INIS)

Sabanov, V.Kh.; Kibizova, A.Yu.; Klimov, E.S.; Berberova, N.T.; Okhlobystin, O.Yu.

1987-01-01

Electrochemical and chemical oxidation of 1,3,1',3'-tetramethyl-2,3,2',3'-tetrahydro-2,2'-dipyriminyl takes place with rupture of the C-C bond in the initially formed cation radical. In the oxidation of the compound with aluminum chloride in nitrobenzene, ESR revealed a cation radical with an unresolved hyperfine structure. Oxidation of the dihydrodimer with nitrosonium perchlorate in nitrobenzene or nitromethane resulted in the same spectra. Cyclic volt-ampere diagrams are included

SYNTHESIS OF 1,2 FUSED SYSTEMS BASED ON THE 3-ARYLIDENE-5-PHENYL-1,2-DIHYDRO-3H-1,4- BENZODIAZEPINE-2-ONES

Directory of Open Access Journals (Sweden)

V. I. Pavlovsky

2014-12-01

Full Text Available By the reaction of 7-bromo-5-aryl-1,2-dihydro-3H-1,4-benzodiazepine-2-ones with Lawesson reagent, 7-bromo-5-aryl-1,2-dihydro-3H-1,4-benzodiazepine-2-tiones were synthesized from which 3-arylidene-7-bromo-2-hydrazino-5-phenyl-3H-1,4-benzodiazepines were obtained by the reaction with hydrazine hydrate. The condensation of 3-arylidene-7-bromo-2-hydrazino-5-phenyl-3H-1,4-benzodiazepines with triethylorthoformate (triethylorthoacetate or formic acid (acetic acid gave 4-arylidene-8-bromo-6-phenyl-4H-[1,2,4]triazolo[4,3-а][1,4]-benzodiazepines. Latter were also synthesized by the reaction of 7-bromo-5-aryl-1,2-dihydro-3H-1,4-benzodiazepine-2-tiones with acetylhydrazine. 4-Arylidene-8-bromo-6-phenyl-4H-[1,2,3,4] tetrazolo[1,5-а][1,4]-benzodiazepines were obtained by the reaction of 3-arylidene-7-bromo-2-hydrazino-5-phenyl-3H-1,4-benzodiazepines with sodium nitrite.

Z-contrast imaging of ordered structures in Pb(Mg1/3Nb2/3)O3 and Ba(Mg1/3Nb2/3)O3

International Nuclear Information System (INIS)

Yan, Y.; Pennycook, S.J.; Xu, Z.; Viehland, D.

1998-02-01

Lead-based cubic perovskites such as Pb(B 1/3 2+ B 2/3 5+ )O 3 (B 2+ Mg, Co, Ni, Zn; B 5+ = Nb, Ta) are relaxor ferroelectrics. Localized order and disorder often occur in materials of this type. In the Pb(Mg 1/3 Nb 2/3 )O 3 (PMN) family, previous studies have proposed two models, space-charge and charge-balance models. In the first model, the ordered regions carry a net negative charge [Pb(Mg 1/2 Nb 1/2 )O 3 ], while in the second model it does not carry a net charge [Pb((Mg 2/3 Nb 1/3 ) 1/2 Nb 1/2 )O 3 ]. However, no direct evidence for these two models has appeared in the literature yet. In this paper the authors report the first direct observations of local ordering in undoped and La-doped Pb(Mg 1/3 Nb 2/3 )O 3 , using high-resolution Z-contrast imaging. Because the ordered structure in Ba(Mg 1/3 Nb 2/3 )O 3 is well known, the Z-contrast image from an ordered domain is used as a reference for this study

Enhancement of electrochemical performance of LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 by surface modification with MnO_2

International Nuclear Information System (INIS)

Guo, Xin; Cong, Li-Na; Zhao, Qin; Tai, Ling-Hua; Wu, Xing-Long; Zhang, Jing-Ping; Wang, Rong-Shun; Xie, Hai-Ming; Sun, Li-Qun

2015-01-01

LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 is successfully coated with MnO_2 by a chemical deposition method. The X-ray diffraction (XRD), scanning electron microscope (SEM) and high resolution transmission electron microscope (HRTEM) results demonstrate that MnO_2 forms a thin layer on the surface of LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 without destroying the crystal structure of the core material. Compared with pristine LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2, the MnO_2-coated sample shows enhanced electrochemical performance especially the rate capability. Even at a current density of 750 mA g"−"1, the discharge capacity of MnO_2-coated LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 is 155.15 mAh g"−"1, while that of the pristine electrode is only 132.84 mAh g"−"1 in the range of 2.5–4.5 V. The cyclic voltammetry (CV) and X-ray photoelectron spectroscopy (XPS) curves show that the MnO_2 coating layer reacts with Li"+ during cycling, which is responsible for the higher discharge capacity of MnO_2-coated LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2. Electrochemical impedance spectroscopy (EIS) results confirmed that the MnO_2 coating layer plays an important role in reducing the charge transfer resistance on the electrolyte–electrode interfaces. - Highlights: • MnO_2 coated LiNi_1_/_3Co_1_/_3Mn_1_/_3O_2 cathode material is synthesized for the first time. • MnO_2 offers available sites for insertion of extracted lithium. • The preserved surface and crystal structures results in the improved kinetics.

Structural and electrical properties of (1-x)(Na1/2Bi1/2)TiO3-xPb(Mg1/3Nb2/3)O3 solid solution

International Nuclear Information System (INIS)

Lee, J.-K.; Yi, J.Y.; Hong, K.S.

2004-01-01

Structural, dielectric and piezoelectric properties of (1-x)(Na 1/2 Bi 1/2 )TiO 3 -xPb(Mg 1/3 Nb 2/3 )O 3 (NBT-xPMN) solid solution have been investigated. An addition of PMN into NBT transformed the structure of sintered samples from rhombohedral to pseudocubic phase where x is larger than 0.1. In calcined powders, however, the intermediate structure were observed between rhombohedral and cubic phases near x=0.1. The formation of solid solution between NBT and PMN modified the dielectric and piezoelectric properties of NBT to be suitable for high temperature dielectric and piezoelectric material. With increasing the content of PMN, the temperature-stability of ε r (T) increased and the high temperature dielectric loss decreased. In addition, the piezoelectric property of NBT-xPMN was enhanced, for the decrease of coercive field and conductivity promoted the domain reversal under the high electric field of the poling process

Crystal structures of 2-methoxyisoindoline-1,3-dione, 1,3-dioxoisoindolin-2-yl methyl carbonate and 1,3-dioxo-2,3-dihydro-1H-benzo[de]isoquinolin-2-yl methyl carbonate: three anticonvulsant compounds

Directory of Open Access Journals (Sweden)

Fortune Ezemobi

2014-12-01

Full Text Available The title compounds, C9H7NO3, (1, C10H7NO5, (2, and C14H9NO5, (3, are three potentially anticonvulsant compounds. Compounds (1 and (2 are isoindoline derivatives and (3 is an isoquinoline derivative. Compounds (2 and (3 crystallize with two independent molecules (A and B in their asymmetric units. In all three cases, the isoindoline and benzoisoquinoline moieties are planar [r.m.s. deviations are 0.021 Å for (1, 0.04 and 0.018 Å for (2, and 0.033 and 0.041 Å for (3]. The substituents attached to the N atom are almost perpendicular to the mean planes of the heterocycles, with dihedral angles of 89.7 (3° for the N—O—Cmethyl group in (1, 71.01 (4 and 80.00 (4° for the N—O—C(=OO—Cmethyl groups in (2, and 75.62 (14 and 74.13 (4° for the same groups in (3. In the crystal of (1, there are unusual intermolecular C=O...C contacts of 2.794 (1 and 2.873 (1 Å present in molecules A and B, respectively. There are also C—H...O hydrogen bonds and π–π interactions [inter-centroid distance = 3.407 (3 Å] present, forming slabs lying parallel to (001. In the crystal of (2, the A and B molecules are linked by C—H...O hydrogen bonds, forming slabs parallel to (10-1, which are in turn linked via a number of π–π interactions [the most significant centroid–centroid distances are 3.4202 (7 and 3.5445 (7 Å], forming a three-dimensional structure. In the crystal of (3, the A and B molecules are linked via C—H...O hydrogen bonds, forming a three-dimensional structure, which is consolidated by π–π interactions [the most significant inter-centroid distances are 3.575 (3 and 3.578 (3 Å].

(2E-1-(3-Chlorophenyl-3-(4-chlorophenylprop-2-en-1-one

Directory of Open Access Journals (Sweden)

Jerry P. Jasinski

2009-11-01

Full Text Available The title compound, C15H10Cl2O, is a chalcone with 3-chlorophenyl and 4-chlorophenyl substituents bonded at the opposite ends of a propenone group, the biologically active region. The dihedral angle between mean planes of these two chloro-substituted benzene rings is 46.7 (7° compared to 46.0 (1 and 32.4 (1° in similar published sructures. The angles between the mean plane of the prop-2-en-1-one group and the mean planes of the 3-chlorophenyl and 4-chlorophenyl rings are 24.1 (2 and 29.63°, respectively. While no classical hydrogen bonds are present, weak intermolecular C—H...π-ring interactions are observed, which contribute to the stability of crystal packing.

1,1′-(Ethane-1,2-diylbis(indoline-2,3-dione

Directory of Open Access Journals (Sweden)

Yao Wang

2010-07-01

Full Text Available The molecule of the title compound, C18H12N2O4, is situated on a crystallographic centre of symmetry. The molecule has a zigzag structure, with two parallel symmetry-related indoline-2,3-dione fragments linked by an ethylene group at each N atom. In the crystal, the molecules stack in columns along the b axis. There are two such columns in the structure. The molecules within each column are parallel; however, the molecules in the two columns differ in the respective orientation of the indoline-2,3-dione fragments. In one column, they are approximately parallel to (112, while in the other they are approximately parallel to (overline{1}12. The interplanar angle between the indoline-2,3-dione fragments in the two columns is 80.83 (3°. The molecules within each column are related by mutual displacement of their centres of symmetry, that is (0, ±1/2, ±1/2. The packing between the molecules is provided by weak interactions only, viz. C—H...O hydrogen bonds and π–π [centroid–centroid distance = 3.8745 (8 Å] and C=O...π interactions.

Ion chemistry of 1H-1,2,3-triazole.

Science.gov (United States)

Ichino, Takatoshi; Andrews, Django H; Rathbone, G Jeffery; Misaizu, Fuminori; Calvi, Ryan M D; Wren, Scott W; Kato, Shuji; Bierbaum, Veronica M; Lineberger, W Carl

2008-01-17

A combination of experimental methods, photoelectron-imaging spectroscopy, flowing afterglow-photoelectron spectroscopy and the flowing afterglow-selected ion flow tube technique, and electronic structure calculations at the B3LYP/6-311++G(d,p) level of density functional theory (DFT) have been employed to study the mechanism of the reaction of the hydroxide ion (HO-) with 1H-1,2,3-triazole. Four different product ion species have been identified experimentally, and the DFT calculations suggest that deprotonation by HO- at all sites of the triazole takes place to yield these products. Deprotonation of 1H-1,2,3-triazole at the N1-H site gives the major product ion, the 1,2,3-triazolide ion. The 335 nm photoelectron-imaging spectrum of the ion has been measured. The electron affinity (EA) of the 1,2,3-triazolyl radical has been determined to be 3.447 +/- 0.004 eV. This EA and the gas-phase acidity of 2H-1,2,3-triazole are combined in a negative ion thermochemical cycle to determine the N-H bond dissociation energy of 2H-1,2,3-triazole to be 112.2 +/- 0.6 kcal mol-1. The 363.8 nm photoelectron spectroscopic measurements have identified the other three product ions. Deprotonation of 1H-1,2,3-triazole at the C5 position initiates fragmentation of the ring structure to yield a minor product, the ketenimine anion. Another minor product, the iminodiazomethyl anion, is generated by deprotonation of 1H-1,2,3-triazole at the C4 position, followed by N1-N2 bond fission. Formation of the other minor product, the 2H-1,2,3-triazol-4-ide ion, can be rationalized by initial deprotonation of 1H-1,2,3-triazole at the N1-H site and subsequent proton exchanges within the ion-molecule complex. The EA of the 2H-1,2,3-triazol-4-yl radical is 1.865 +/- 0.004 eV.

Synthesis and Antibacterial Activities of Novel 2,5-Diphenylindolo[2,3-e] Pyrazolo[1',5':3",4"]pyrimido[2",1"-c] [1,2,4]triazines

Directory of Open Access Journals (Sweden)

Mohamed G. Marei

2011-12-01

Full Text Available The formation of (E-3-{2-(2,5-diphenylpyrazolo[1,5-c]pyrimidin-7-ylhydrazono}indolin-2-ones 3 has been achieved by condensation of equimolar amounts of 7-hydrazino-2,5-diphenylpyrazolo[1,5-c]pyrimidine (1 and isatin (or isatin derivatives 2 at room temperature. The (E-products could be isomerized into corresponding the (Z-3 isomers. Reactions of the latter fused heterocyclic hydrazones towards different electro-philic reagents yielded the corresponding 3-substituted derivatives 4–7. Dehydrative cyclisation of the hydrazones 3 using phosphorus oxychloride afforded the 2,5-diphenyl- indolo[2,3-e]pyrazolo[1',5':3",4"]pyrimido[2",1"-c][1,2,4] triazines 13. The polyfused heterocyclic ring system 13 underwent electrophilic substitution reactions at position 4 rather than at position 3. The 3-bromo isomer of 17 was prepared by a sequence of reactions starting from 2,5-diphenylpyrazolo[1,5-c]pyrimidine-7(6H-thione (11. The orientation of the electrophilic attack was supported by spectroscopic and chemical evidence. Some of the synthesized compounds were found to possess slight to moderate activity against the microorganisms Bacillus subtilis, Micrococcus luteus, Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa.

Microwave assisted synthesis and antimicrobial activity of novel 1-[1/2-(1-Benzyl-1H-[1,2,3]triazol-4-ylmethoxy-naphthalen-2/1-yl]-3-(1-phenyl-3-aryl-1H-pyrazol-4-yl-propenones

Directory of Open Access Journals (Sweden)

Dongamanti Ashok

2015-06-01

Full Text Available A series of novel 1-[1/2-(1-Benzyl-1H-[1,2,3]triazol-4-ylmethoxy-naphthalen-2/1-yl]-3-(1-phenyl-3-aryl-1H-pyrazol-4-yl-propenones were design and synthesized by Click reaction followed by Claisen-Schmidt condensation under microwave irradiation and conventional heating methods. The structures of newly synthesized compounds have been established on the basis of elemental analysis, IR, 1H & 13C NMR and mass spectral data. All the compounds were screened for their antimicrobial activity.

Butane-1,2,3,4-tetracarboxylic acid–1,10-phenanthroline–water (1/2/2

Directory of Open Access Journals (Sweden)

Hong-lin Zhu

2011-07-01

Full Text Available The asymmetric unit of the title compound, 2C12H8N2·C8H10O8·2H2O, contains one 1,10-phenanthroline molecule, one half-molecule of butane-1,2,3,4-tetracarboxylic acid (H4BTC and a water molecule, with the complete tetra-acid generated by crystallographic inversion symmetry. Intermolecular O—H...O hydrogen bonds and π–π stacking interactions [centroid–centroid distances = 3.672 (2 and 3.708 (2 Å form an extensive three-dimensional network, which consolidates the crystal packing.

Synthesis of fused 1,2,4-dithiazines and 1,2,3,5-trithiazepines.

Science.gov (United States)

Koyioni, Maria; Manoli, Maria; Koutentis, Panayiotis A

2014-10-17

Reacting (Z)-N-(4-chloro-5H-1,2,3-dithiazol-5-ylidene)-1H-pyrazol-5-amines 5 with Et2NH and then with concd H2SO4 gives 5H-pyrazolo[3,4-e][1,2,4]dithiazine-3-carbonitriles 7 in good yields (74-85%) and 6H-pyrazolo[3,4-f][1,2,3,5]trithiazepine-4-carbonitriles 9 as minor products (0-6%). Furthermore, the 1,3-dimethylpyrazole analogue 5a was transformed into the dithiazine 7a in two discrete steps, allowing the isolation of a disulfide intermediate (Z)-2-[(diethylamino)disulfan-yl]-2-[(1H-pyrazol-5-yl)imino]acetonitrile (8a). The one-pot, two-step reaction also worked with electron-rich hydroxy- and methoxy-substituted anilines. Thermolysis of the pyrazolo[3,4-e][1,2,4]dithiazines 7 gave the ring-contracted 1H-pyrazolo[3,4-d]thiazole-5-carbonitriles 6 (94-100%). With active sulfur, 1,3-dimethyl-5H-pyrazolo[3,4-e][1,2,4]dithiazine-3-carbonitrile (7a) gave 1,3-dimethyl-6H-pyrazolo[3,4-f][1,2,3,5]trithiazepine-4-carbonitrile (9a), but on prolonged reaction times, it gave 5,7-dimethyl-5H-[1,2,3]dithiazolo[4,5-b]pyrazolo[3,4-e][1,4]thiazine (13). Finally, in the absence of acid, heating a solution of (Z)-2-[(diethylamino)disulfanyl]-2-[(1,3-dimethyl-1H-pyrazol-5-yl)imino]acetonitrile (8a) gave 4,6,10,12-tetramethyl-6H-pyrazolo[3,4-f]pyrazolo[3',4':4,5]pyrimido[6,1-d][1,2,3,5]trithiazepine-8,12b(10H)-dicarbonitrile (19) (67%).

Synthesis of 1-amino-2-[3-(3-[2,6-14C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3,4-dione hydrochloride

International Nuclear Information System (INIS)

Swigor, J.E.; Algieri, A.A.; Standridge, R.T.; Pittman, K.A.

1985-01-01

The synthesis of the title compound is described. The condensation of 3-aminopropanol with phthalic anhydride and subsequent treatment with phosphorous tribromide produced N-[3-bromopropyl] phthalimide. Acylation with 3-hydroxybenzaldehyde, reduction with hydrogen over Raney nickel and subsequent treatment with thionyl chloride gave N-[3-(3-chloromethylphenoxy) propyl] phthalimide. Treatment with [2,6 - 14 C] piperidine introduced the radiolabel. Deprotection of the amino group with hydrazine and treatment with 3-methoxy-4-amino-3-cyclobutene-1,2-dione produced 1-amino-2-[3-(3-[2,6- 14 C]piperidinomethylphenoxy) propylamino]-1-cyclobutene-3, 4-dione. Treatment with hydrochloric acid yielded the title compound in an overall chemical yield of 22%. (author)

(E-3-Methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone

Directory of Open Access Journals (Sweden)

Yordanka Ivanova

2016-04-01

Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(thiophen-2-yl-1-propenyl-2(3H-benzothiazolone, was synthesized by Claisen-Schmidt condensation of 3-methyl-2(3H-benzothiazolone-6-carbaldehyde with 2-acetylthiophene in 94% yield. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.

The 1:1 adduct of caffeine and 2-(1,3-dioxoisoindolin-2-ylacetic acid

Directory of Open Access Journals (Sweden)

Moazzam H. Bhatti

2011-09-01

Full Text Available In the crystal structure of the title adduct [systematic name: 2-(1,3-dioxoisoindolin-2-ylacetic acid–1,3,7-trimethyl-1,2,3,6-tetrahydro-7H-purine-2,6-dione (1/1], C8H10N4O2·C10H7NO4, the components are linked by an O—H...N hydrogen-bond and no proton transfer occurs.

Crystal structures of nitrato-(2-[2-(1-pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) aquacopper and chloro-(2-[2-phenyl(pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) copper

Energy Technology Data Exchange (ETDEWEB)

Chumakov, Yu. M. [Academy of Sciences of Moldova, Institute of Applied Physics (Moldova, Republic of); Paholnitcaia, A. Yu. [State University of Moldova (Moldova, Republic of); Petrenko, P. A. [Academy of Sciences of Moldova, Institute of Applied Physics (Moldova, Republic of); Tsapkov, V. I., E-mail: vtsapkov@gmail.com [State University of Moldova (Moldova, Republic of); Poirier, D. [Centre Hospitalier Universitaire de Quebec (Canada); Gulea, A. P. [State University of Moldova (Moldova, Republic of)

2015-01-15

Two crystal modifications of nitrato-(2-[2-(1-pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) aquacopper (I and II) and two modifications of chloro-(2-[2-phenyl(pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) copper (III and IV) have been synthesized and studied by X-ray diffraction. In structures I and II, the copper atoms coordinate a monodeprotonated molecule of the organic ligand, nitrate ions, and a water molecule. In crystals of I, the complexes are monomeric, whereas complexes II are linked via nitrate ions to form polymeric chains. In both structures the coordination polyhedron of the copper atom can be described as a distorted tetragonal bipyramid—(4 + 1 + 1) in I and (4 + 2) in II. These coordination polyherdra have different compositions. In structures III and IV, the metal atoms coordinate a monodeprotonated (2-[2-phenyl(pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazole molecule and chloride ions. In III the complex-forming ion has square-planar coordination geometry, whereas structure IV consists of centrosymmetric dimers with two bridging chlorine atoms. It was found that nitrato-(2-[2-(1-pyridine-2-ylethylidene)hydrazine]-1,3-benzothiazolo) aquacopper possesses antitumor activity.

(E-1-(2-Bromophenyl-3-(2,5-dimethoxyphenylprop-2-en-1-one

Directory of Open Access Journals (Sweden)

Jerry P. Jasinski

2010-08-01

Full Text Available The title compound, C17H15BrO3, is a chalcone with the 2-bromophenyl and 2,5-dimethoxyphenyl rings bonded at opposite ends of a propene group. The dihedral angle between the mean planes of the ortho-bromo and ortho,meta-dimethoxy-substituted benzene rings is 77.3 (1°. The dihedral angles between the mean plane of the prop-2-ene-1-one group and the mean planes of the 2-bromophenyl and 2,5-dimethoxyphenyl rings are 58.6 (1 and 30.7 (4°, respectively. Weak C—H...O, C—H...Br and π–π stacking intermolecular interactions [centroid–centroid distance = 3.650 (2 Å] are present in the structure.

1,5-Dimethyl-2-phenyl-1H-pyrazol-3(2H-one–4,4′-(propane-2,2-diylbis[1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one] (1/1

Directory of Open Access Journals (Sweden)

Krzysztof Lyczko

2013-01-01

Full Text Available The asymmetric unit of the title compound, C11H12N2O·C25H28N4O2, contains two different molecules. The smaller is known as antipyrine [systematic name: 1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one] and the larger is built up from two antypirine molecules which are connected through a C atom of the pyrazolone ring to a central propanyl part [systematic name: 4,4′-(propane-2,2-diylbis[1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one]. Intramolecular C—H...O hydrogen bonds occur in the latter molecule. In the crystal, C—H...O hydrogen bonds link the molecules into a two-dimensional network parallel to (001.

Thermodynamic study of 1,2,3-triphenylbenzene and 1,3,5-triphenylbenzene

International Nuclear Information System (INIS)

Ribeiro da Silva, Manuel A.V.; Santos, Luis M.N.B.F.; Lima, Luis M. Spencer S.

2010-01-01

The energetic study of 1,2,3-triphenylbenzene (1,2,3-TPhB) and 1,3,5-triphenylbenzene (1,3,5-TPhB) isomers was carried out by making use of the mini-bomb combustion calorimetry and Knudsen mass-loss effusion techniques. The mini-bomb combustion calorimetry technique was used to derive the standard (p o = 0.1 MPa) molar enthalpies of formation in the crystalline state from the measured standard molar energies of combustion for both isomers. The Knudsen mass-loss effusion technique was used to measure the dependence with the temperature of the vapour pressure of crystalline 1,2,3-TPhB, which allowed the derivation of the standard molar enthalpy of sublimation, by application of the Clausius-Clapeyron equation. The sublimation study of 1,3,5-TPhB had been performed previously. From the combination of data obtained by both techniques, the standard molar enthalpies of formation in the gaseous state, for both isomers, at T = 298.15 K, were calculated. The results indicate a higher stability of the 1,3,5-TPhB isomer relative to 1,2,3-TPhB, similarly to the terphenyls. Nevertheless, the 1,2,3-TPhB isomer is not as energetically destabilized as one might expect, supporting the existence of a π-π displacive stacking interaction between both pairs of outer phenyl rings. The volatility difference between the two isomers is ruled by the enthalpy of sublimation. The volatility of the 1,2,3-TPhB is two orders of magnitude higher than the 1,3,5-TPhB isomer, at T = 298.15 K.

Dipropyl 3,6-diphenyl-1,2-dihydro-1,2,4,5-tetrazine-1,2-dicarboxylate.

Science.gov (United States)

Rao, Guo-Wu; Hu, Wei-Xiao

2003-05-01

The title compound, C(22)H(24)N(4)O(4), was prepared from propyl chloroformate and 3,6-diphenyl-1,2-dihydro-s-tetrazine. This reaction yields the title compound rather than dipropyl 3,6-diphenyl-1,4-dihydro-s-tetrazine-1,4-dicarboxylate. The 2,3-diazabutadiene group in the central six-membered ring is not planar; the C=N double-bond length is 1.285 (2) A, and the average N-N single-bond length is 1.401 (3) A, indicating a lack of conjugation. The ring has a twist conformation, in which adjacent N atoms lie +/- 0.3268 (17) A from the plane of the ring. The molecule has twofold crystallographic symmetry.

Synthesis, crystal structure, and spectra of 3,3- dimethyl-1-N-(1'-phenyl-2',3'-dimethyl-5'-oxo-3'- pyrazolin-4'-yl)imino-1,2,3,4-tetrahydroisoquinoline

International Nuclear Information System (INIS)

Sokol, V.I.; Ryabov, M.A.; Merkur'eva, N.Yu.; Davydov, V.V.; Zaitsev, B.E.; Shklyaev, Yu.V.; Sergienko, V.S.; Zaitsev, B.E.

1996-01-01

The synthesis and the crystal and molecular structure of 3,3-dimethyl-1-N-(1'-phenyl-2',3'- dimethyl-5'-oxo-3'-pyrazolin-4'-yl)imino-1,2,3,4-tetrahydroisoquinoline are reported. As is evidenced by the 1H NMR, IR, and electron spectra, the tautomeric form of the compounds observed in the crystal is also retained in solutions

Synthesis of some novel 4-aza-tricyclo[5.2.2.0 2,6 ]undecane-3,5,8-triones from 2-trimethylsilyloxy-1,3-cyclohexadiene and 1-methoxy-1,3-cyclohexadiene

Directory of Open Access Journals (Sweden)

Hosapalya Thimmaiah Srinivasa

2012-01-01

Full Text Available The synthesis and characterization of nine novel Diels-Alder cycloadducts: the 4-aza-tricyclo[5.2.2.0 2,6] undecane-3,5,8-triones using 2-trimethylsilyloxy-1,3-cyclohexadiene and 1-methoxy-1,3-cyclohexadiene is reported. The isolated yields of the pure cycloadducts range between 75 to 95%.

2-(3-Methylphenyl-1,2-benzoselenazol-3(2H-one

Directory of Open Access Journals (Sweden)

Liyun Wang

2017-04-01

Full Text Available In the title ebselen derivative, C14H11NOSe, the nine-membered benzisoselenazolyl ring system is approximately planar (r.m.s. deviation = 0.021 Å. The dihedral angle between its mean plane and that of the 3-methylphenyl ring is 5.37 (11°. The five-membered isoselenazolyl ring is severely strained at the Se atom: Se—N = 1.889 (2 Å, Se—Car = 1.882 (3 Å and N—Se—Car = 83.30 (10°. In the crystal, molecules are linked by C—H...O hydrogen bonds and short intermolecular Se...O contacts of 2.6917 (19 Å, forming chains along the c-axis direction. Neighbouring molecules are linked by offset π–π interactions [intercentroid distance = 3.535 (2 Å]. The chains are also linked by C—H...π interactions, forming a three-dimensional structure.

(2E-3-(6-Chloro-2-methoxyquinolin-3-yl-1-(2-methyl-4-phenylquinolin-3-ylprop-2-en-1-one acetone monosolvate

Directory of Open Access Journals (Sweden)

Edward R. T. Tiekink

2013-08-01

Full Text Available In the title solvate, C29H21ClN2O2·C3H6O, a prop-2-en-1-one bridge links two quinolinyl residues; the latter are almost perpendicular [dihedral angle = 78.27 (6°]. The dihedral angle between the quinonyl ring system and its pendant phenyl group is 59.78 (8°. A small twist in the bridging prop-2-en-1-one group is noted [O=C—C=C torsion angle = −10.6 (3°]. In the crystal, a three-dimensional architecture arises as a result of C—H...O and π–π stacking [centroid–centroid distances = 3.5504 (12–3.6623 (12 Å].

Optically active antifungal azoles. XII. Synthesis and antifungal activity of the water-soluble prodrugs of 1-[(1R,2R)-2-(2,4-difluorophenyl)-2-hydroxy-1-methyl-3-(1H-1,2,4-triazol-1-yl)propyl]-3-[4-(1H-1-tetrazolyl)phenyl]-2-imidazolidinone.

Science.gov (United States)

Ichikawa, T; Kitazaki, T; Matsushita, Y; Yamada, M; Hayashi, R; Yamaguchi, M; Kiyota, Y; Okonogi, K; Itoh, K

2001-09-01

1-[(1R,2R)-2-(2,4-Difluorophenyl)-2-hydroxy-1-methyl-3-(1H-1,2,4-triazol-1-yl)propyl]-3-[4-(1H-1-tetrazolyl)phenyl]-2-imidazolidinone (1: TAK-456) was selected as a candidate for clinical trials, but since its water-solubility was insufficient for an injectable formulation, the quaternary triazolium salts 2 were designed as water-soluble prodrugs. Among the prodrugs prepared, 4-acetoxymethyl-1-[(2R,3R)-2-(2,4-difluorophenyl)-2-hydroxy-3-[2-oxo-3-[4-(1H-1-terazolyl)phenyl]-1-imidazolidinyl]butyl]-1H-1,2,4-triazolium chloride (2a: TAK-457) was selected as an injectable candidate for clinical trials based on the results of evaluations on solubility, stability, hemolytic effect and in vivo antifungal activities.

Analogues of the muscarinic agent 2'-methylspiro[1-azabicyclo[2.2.2]octane-3,4'-[1,3]dioxolane]: synthesis and pharmacology.

Science.gov (United States)

Nordvall, G; Sundquist, S; Glas, G; Gogoll, A; Nilvebrant, L; Hacksell, U

1992-05-01

A number of tetrahydrofuran analogues of 2'-methylspiro[1-azabicyclo[2.2.2]octane-3,4'-[1,3]dioxolane] (1) have been prepared with the aim to obtain information about the relative importance of each of the oxygens in 1 for efficacy and for selectivity. In addition, the dimethyl and desmethyl analogues of 1 were prepared. The new compounds were compared to cis- and trans-1 with regard to their ability to displace (-)-[3H]-3-quinuclidinyl benzilate ((-)-[3H]QNB) from muscarinic receptors in cerebral cortex, heart, parotid gland, and urinary bladder from guinea pigs. Functional studies were made on isolated guinea pig bladder and ileum. The new compounds exhibited both lower affinity and efficacy than cis-1. A conformational study was performed, and the effects of steric and electronic factors on the biological activity of the compounds are discussed.

Electric Properties of Pb(Sb1/2Nb1/2)O3 PbTiO3 PbZrO3 Ceramics

Science.gov (United States)

Kawamura, Yasushi; Ohuchi, Hiromu

1994-09-01

Solid-solution ceramics of ternary system xPb(Sb1/2Nb1/2)O3 yPbTiO3 zPbZrO3 were prepared by the solid-state reaction of powder materials. Ceramic, electric, dielectric and piezoelectric properties and crystal structures of the system were studied. Sintering of the system xPb(Sb1/2Nb1/2)O3 yPbTiO3 zPbZrO3 is much easier than that of each end composition, and well-sintered high-density ceramics were obtained for the compositions near the morphotropic transformation. Piezoelectric ceramics with high relative dielectric constants, high radial coupling coefficient and low resonant resistance were obtained for the composition near the morphotropic transformation. The composition Pb(Sb1/2Nb1/2)0.075Ti0.45Zr0.475O3 showed the highest dielectric constant (ɛr=1690), and the composition Pb(Sb1/2Nb1/2)0.05Ti0.45Zr0.5O3 showed the highest radial coupling coefficient (kp=64%).

2-(2,4-Dichlorophenyl-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylacetamide

Directory of Open Access Journals (Sweden)

B. Narayana

2013-01-01

Full Text Available In the crystal structure of the title compound, C19H17Cl2N3O2, the molecules form dimers of the R22(10 type through N—H...O hydrogen bonding. As a result of steric repulsion, the amide group is rotated with respect to both the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings, making dihedral angles of 80.70 (13 and 64.82 (12°, respectively. The dihedral angle between the dichlorophenyl and 2,3-dihydro-1H-pyrazol-4-yl rings is 48.45 (5° while that between the 2,3-dihydro-1H-pyrazol-4-yl and phenyl rings is 56.33 (6°.

Synthesis of 1-13C-1-indanone and 2-13C-1,2,3,4-tetrahydroquinoline

International Nuclear Information System (INIS)

Pickering, R.E.; Wysocki, M.A.; Eisenbraun, E.J.

1985-01-01

The synthesis of 2- 13 C-1,2,3,4-tetrahydroquinoline (5) via 1- 13 C-3-phenylpropanoic acid (1), 1- 13 C-1-indanone (2), 1- 13 C-1-indanone hydrazone (3) and 2- 13 C-3,4-dihydro-2(1H)-quinolinone (4) proceeded in 78, 96, 95, 79, and 85% individual yields respectively for 1, 2, 3, 4, 5 and 61% overall yield of the latter from 1. (author)

Synthesis of aryl-1H-1,2,3-triazoles via 1,3-dipolar cycloaddition

Directory of Open Access Journals (Sweden)

Wagner O. Valença

2012-06-01

Full Text Available A series of Aryl-1H-1,2,3-triazoles were prepared from the reaction between aril-azide (1 with 1.5 equiv. of terminal alkynes (2a-o. The reactions carried out at room temperature and in the presence of CuI (10 mol% in acetonitrile. The compounds (3a-o were obtained in moderate-to-good yields (50-94%. In general, not was observed significant inductive effect on the reactivity of the alkynes (2a-f. The alcohol alkynes (2i-k showed moderate yields 50-72%. On the other hand, the reaction with alkyl alkynes (2m,n furnished the compounds (3m and (3n in excellent yields of 89% and 90%, respectively.

1-(2-Chlorobenzyloxy-3-[1,2,3]triazol-1-yl-propan-2-ol Derivatives: Synthesis, Characterization, and DFT-Based Descriptors Analysis

Directory of Open Access Journals (Sweden)

Eloisa Román-Maldonado

2017-01-01

Full Text Available A novel series of 1-(2-chlorobenzyloxy-3-[1,2,3]triazol-1-yl-propan-2-ol derivatives was designed and synthesized using copper catalyzed alkyne-azide cycloaddition in the key step. Theoretical investigation of molecular and electronic properties by means of global and local reactivity indexes of the synthetized compounds was carried out, using DFT (Density Functional Theory at PBEPBE/6-31++G⁎⁎ level.

7-{[2-(4-Hydroxyphenylmethylidene]amino}-1,3-thiazol-4-yl-2-(methoxyiminoacetyl]amino}-3-{[(2-methyl-5,6-dioxo-1,2,5,6-tetrahydro-1,2,4-triazin-3-ylsulfanyl]methyl}-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic Acid

Directory of Open Access Journals (Sweden)

Ghulam Fareed

2012-05-01

Full Text Available Novel 7-{[2-(4-hydroxyphenylmethylidene]amino}-1,3-thiazol-4-yl-2-(methoxyiminoacetyl]amino}-3-{[(2-methyl-5,6-dioxo-1,2,5,6-tetrahydro-1,2,4-triazin-3-ylsulfanyl]methyl}-8-oxo-5-thia-1azabicyclo [4.2.0]oct-2-ene-2-carboxylic acid was prepared by condensation of ceftriaxone disodium (1 with 4-hydroxybenzaldehyde (2 in ethanol under reflux conditions for 3–4 h. The structure of synthesized compound was elucidated using LCMS, ¹H-NMR, and CHN techniques.

Crystal structures of three 1-oxo-1,2-dihydronaphthalene derivatives: dimethyl 4-(4-methoxyphenyl-2-(4-methylphenyl-1-oxo-1,2-dihydronaphthalene-2,3-dicarboxylate, dimethyl 1-oxo-2-(pyren-4-yl-4-(thiophen-2-yl-1,2-dihydronaphthalene-2,3-dicarboxylate and ethyl 1-oxo-2-phenyl-2,4-bis(thiophen-2-yl-1,2-dihydronaphthalene-3-carboxylate

Directory of Open Access Journals (Sweden)

S. Gopinath

2017-02-01

Full Text Available In the title 1-oxo-1,2-dihydronaphthalene derivatives, C28H24O6, (I, C34H22O5S, (II, and C27H20O3S2, (III, the cyclohexa-1,3-diene rings of the 1,2-dihydronaphthalene ring systems adopt half-chair, boat and half-chair conformations, respectively. The carbonyl O atoms attached to the dihydronaphthalene ring systems are each significantly deviated from the mean plane of the 1,2-dihydronaphthalene ring system, by 0.6162 (12 Å in (I, 0.6016 (16 Å in (II and 0.515 (3 Å in (III. The mean planes of the 1,2-dihydronaphthalene ring systems make dihedral angles of 85.83 (3, 88.19 (3 and 81.67 (8°, respectively, with the methylphenyl ring in (I, the pyrene ring in (II and the phenyl ring in (III. In (I, the molecular structure is stabilized by an intramolecular C—H...O hydrogen bond, generating an S(6 ring motif. In the crystal of (I, molecules are linked by an intermolecular C—H...O hydrogen bond, which generates a C(8 zigzag chain running along [100]. Adjacent chains are further connected by C—H...π and offset π–π interactions [centroid–centroid distance = 3.6572 (9 Å], forming a double-chain structure. In the crystals of (II and (III, molecules are linked into chain structures by offset π–π interactions with centroid–centroid distances of 3.5349 (12 and 3.8845 (13 Å for (II and 3.588 (2 Å for (III. In (II and (III, the thiophene rings are orientationally disordered over two sites, with occupancy ratios of 0.69:0.31 for (II, and 0.528 (4:0.472 (4 and 0.632 (5:0.368 (5 for (III.

Evaluation excitation functions for "2"8Si(n,p)"2"8Al, "3"1P(n,p)"3"1Si, and "1"1"3In(n,γ)"1"1"4"mIn reactions

International Nuclear Information System (INIS)

Zolotarev, K.I.

2014-10-01

Cross section data for "2"8Si(n,p)"2"8Al, "3"1P(n,p)"3"1Si and "1"1"3In(n,γ)"1"1"4"mIn reactions are needed for solving a wide spectrum of scientific and technical tasks. The excitation function of "2"8Si(n,p)"2"8Al reaction refers to the nuclear data involved in fusion reactor design calculations. The "2"8Si(n,p)"2"8Al reaction is interesting also as the monitor reaction for measurements at fusion facilities. Activation detectors on the basis of the 31P(n,p)31Si reaction are commonly used in the reactor dosimetry. The "1"1"3In(n,γ)"1"1"4"mIn reaction is promising regarding reactor dosimetry application for two reasons. First, due to the "1"1"4"mIn decay parameters which are rather suitable for activation measurements. Half-life of "1"1"4"mIn is equal to T_1/_2 = (49.51 ± 0.01) days and gamma spectrum accompanying decay has only one line with energy 190.27 keV and intensity (15.56 ± 0.15)%. Second, the "1"1"3In(n,γ)"1"1"4"mIn reaction rate may be measured by using one activation detector simultaneously with the "1"1"5In(n,γ)"1"1"6"mIn reaction. Preliminary analysis of existing evaluated excitation functions for "2"8Si(n,p)"2"8Al, "3"1P(n,p)"3"1Si and "1"1"3In(n,γ)"1"1"4"mIn reactions show that new evaluations are needed for all above mentioned reactions. This report is devoted to the preparation of the new evaluations of cross sections data and related covariance matrixes of uncertainties for the "2"8Si(n,p)"2"8Al, "3"1P(n,p)"3"1Si and "1"1"3In(n,γ)"1"1"4"mIn reactions.

Main metabolites of 1-(2-chloroethyl)-3-[1'-(5'-p-nitrobenzoyl-2',3'-isopropylidene)-alpha, beta-D-ribofuranosyl]-1-nitrosourea and 1-(2-chloroethyl)-3-(2',3', 4'-tri-O-acetyl-alpha, beta-D-ribopyranosyl)-1-nitrosourea in rats

International Nuclear Information System (INIS)

Madelmont, J.C.; Moreau, M.F.; Godeneche, D.; Duprat, J.; Plagne, R.; Meyniel, G.

1982-01-01

The metabolism of two glycosylnitrosoureas, 1-(2-chloroethyl)-3-[1'-(5'-p-nitrobenzoyl-2',3'-isopropylidene)-alpha, beta-D-ribofuranosyl]-1-nitrosourea (RFCNU) and 1-(2-chloroethyl)-3-(2',3',4'-tri-O-acetyl-alpha, beta-D-ribopyranosyl)-1-nitrosourea (RPCNU), has been investigated in the rat. With the label on the carboxyl moiety of RFCNU, we have shown that hydrolysis of the 4-nitrobenzoyl ester occurred to a large extent in vivo; 4-nitrobenzoic acid and its glucuronide were the major urinary metabolites. Two other minor metabolites and their glucuronides were identified as 4-aminobenzoic acid and 4-acetamidobenzoic acid. With the label on the chloroethyl moieties of RFCNU and RPCNU, we have shown that chloroethanol was a major degradation product of this alkylating part of the molecule. The concentration of chloroethanol in plasma vs. time has been determined. In urine, four metabolites derived from alkylated glutathione, namely thiodiacetic acid and its sulfoxide, N-acetylcarboxymethylcysteine, and N-acetylhydroxyethylcysteine, have been identified

Identifikasi Secara Serologi Galur Virus Flu Burung Subtipe H5N1 Clade 2.1.3 dan Clade 2.3.2 pada Ayam Petelur (SEROLOGICAL IDENTIFICATION OF AVIAN INFLUENZA STRAIN VIRUS SUBTYPE H5N1 CLADE 2.1.3 AND CLADE 2.3.2 FROM LAYER

Directory of Open Access Journals (Sweden)

Aprilia Kusumastuti

2015-10-01

Full Text Available The aim of the study was to know avian influenza (AI infection in field by using serology test in threemarketing area of AI vaccines. Haemagglutination inhibition methode was used in this test. There werefour antigen strains of AI subtype H5N1 clade 2.1.3 (AIstrainA/Chicken/West Java/PWT-WIJ/2006, AIstrain A/Chicken/Garut/BBVW-223/2007, AI strain A/Chicken/West Java-Nagrak/30/2007, and AI strainA/Chicken/Pekalongan/BBVW-208/2007 and 2 antigen strains of AI subtype H5N1 clade 2.3.2 (AI strainA/duck/Sukoharjo/BBVW-1428-9/2012 and AI strain A/duck/Sleman/BBVW-1463-10/2012 was used inthis study for HI test. The result presents that 93,33% chicken farms in three marketing area of PT. SanbioLaboratories have positive antibody titre to AI subtype H5N1 clade 2.1.3. This titre may be obtained fromAI clade 2.1.3 vaccination. From 15 samples, 92,86% are positive to AI subtype H5N1 clade 2.3.2A/duck/Sukoharjo/BBVW-1428-9/2012 and 92,31% are positive to A/duck/Sleman/BBVW-1463-10/2012 evenwithout AI clade 2.3.2 vaccination. This antibody titre may be obtained from AI clade 2.1.3 vaccine crossprotection or field infection.

The preparation of 3-aminoxy-1-amino[1,1'-3H2]propane

International Nuclear Information System (INIS)

Pankaskie, M.C.; Scholtz, S.J.

1989-01-01

3-Aminoxy-1-aminopropane (APA) has previously been shown to be a potent inhibitor of the polyamine biosynthesis enzymes ornithine decarboxylase, adenosylmethionine decarboxylase, and spermidine synthase. Little information is known, however, regarding its mechanism of action, binding site mode(s), or cellular distribution. This report presents a relatively simple three step synthesis of 3-aminoxy-1-amino[1,1'- 3 H 2 ]propane via the catalytic tritiation of 3-aminoxypropionitrile hydrochloride. (author)

Synthesis of (R)-5-(Di[2,3-3H2]propylamino)-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one-([3H]U-86170) and (R)-5-([2,3-3H2]propylamino)-5,6-dihydro-4H-imidazo(4,5,1-ij) quinolin-2(1H)-one ([3H]U-91356)

International Nuclear Information System (INIS)

Moon, M.W.; Hsi, R.S.P.

1992-01-01

(R)-5-(diallylamino)-5,6-dihydro-4H-imidazo[4,5,1-ij]quinolin-2(1H)-one (12b) was prepared in 9% overall yield from 3-aminoquinoline. Reaction of 12b in ethyl acetate with tritium gas in presence of a 5% platinum on carbon catalyst afforded a mixture of (R)-5-(di[2,3- 3 H 2 ]propylamino)-5,6-dihydro-4H-imidazo[4,5,1-ij]-quinolin-2(1H)-one ([ 3 H]U-86170, 69 Ci/mmol) and (R)-5-([2,3- 3 H 2 ]-propylamino)5,6-dihydro-4H-imidazo-[4,5,1-ij]quinolin-2(1H)-one ( [ 3 H]U-91356, 34 Ci/mmol) which was separated by preparative reverse-phase chromatography. U-86170 and U-91356 are potent dopamine D2 agonists. The labelled compounds are useful for drug disposition studies. [ 3 H]U-86170 is also useful as a dopamine D2 agonist radioligand for receptor binding studies. (author)

Synthesis of (R,S)-[2,3-13C2]-1-(1'-methyl-2'-pyrrolidinyl)propan-2-one; {(R,S)-[2',3'-13C2]hygrinePound right bracePound

International Nuclear Information System (INIS)

Abraham, T.W.; Leete, Edward

1996-01-01

2-Ethoxy-1-methyl-5-pyrrolidinone (1) was reacted with ethyl [3,4- 13 C 2 ]-acetoacetate (2) in the presence of TiCl 4 to give ethyl [3,4- 13 C 2 ]-2-(1'-methyl-5'-oxo-2'-pyrrolidinyl)-3-oxobutanoate (3) in 85% yield. Decarboethoxylation of ethyl [3,4- 13 C 2 ]-2-(1'-methyl-5'-oxo-2'-pyrrolidinyl)-3-oxobutan-oate (3) was accomplished using NaCl and H 2 O in DMSO to give (R,S)-[2,3- 13 C 2 ]-1-(1'-methyl-5'-oxo-2'-pyrrolidinyl)propan-2-o ne (4) in 91% yield. Protection of the ketone as a ketal (ethylene glycol, H + ), followed by reduction of the amide to the amine using LiAlH 4 and subsequent deprotection of the ketal gave (R,S)-[2,3- 13 C 2 ]-1-(1'-methyl-2'-pyrrolidinyl)propan-2-one ((R,s)-[2', 3'- 13 C 2 ]Hygrine) (8) in 78% yield. (61% overall yield from ethyl [3,4- 13 C 2 ]acetoacetate). (Author)

Stress relaxation of La1/2Sr1/2MnO3 and La2/3Ca1/3MnO3 at solid oxide fuel cell interfaces

International Nuclear Information System (INIS)

Lussier, A.; Dvorak, J.; Stadler, S.; Holroyd, J.; Liberati, M.; Arenholz, E.; Ogale, S.B.; Wu, T.; Venkatesan, T.; Idzerda, Y.U.

2008-01-01

Interfacial stress is thought to have significant effects on electrical and oxygen transport properties in thin films of importance in solid oxide fuel cell applications. We investigate how in-plane biaxial stress modifies the electronic structure of La 2/3 Ca 1/3 MnO 3 and La 1/2 Sr 1/2 MnO 3 thin films prepared by pulsed laser deposition on three different substrates to vary the in-plane stress from tensile to compressive. The electronic structure was probed by X-ray absorption spectroscopy of the Mn L 2,3 -edge to characterize the interfacial disruption in this region in an element-specific, site-specific manner. The compressive or tensile interfacial strain modifies the relative concentrations of La and Sr in the interfacial region in order to achieve a better lattice match to the contact material. This atomic migration generates an interfacial region dominated by a compound with a single valency for the transition metal ion, resulting in a severe barrier to oxygen and electron transport through this region

Amino methylation of 2-R-6-R_1-imidazo-[2.1-B]-1.3.4-thiadiazole

International Nuclear Information System (INIS)

Saidov, D.K.; Rakhmonov, R.O.; Khodzhiboev, Yu.; Kukaniev, M.A.; Bandaev, S.

2015-01-01

Present article is devoted to amino methylation of 2-R-6-R_1-imidazo-[2.1-B]-1.3.4-thiadiazole. The reaction of new modifications of derivatives of imidazo-[2.1-B]-1.3.4-thiadiazoles-2-bromine-6-p-bromophenyl and 2-alkyl alkylene sulfonyl-6-phenyl imidazo--[2.1-B]-1.3.4-thiadiazole on Mannich with secondary and heterocyclic amines was studied.

Local atomic characterization of LiCo1/3Ni1/3Mn1/3O2 cathode material

International Nuclear Information System (INIS)

Nedoseykina, Tatiana; Kim, Sung-Soo; Nitta, Yoshiaki

2006-01-01

Co, Ni and Mn K-edge XAFS investigation of LiCo 1/3 Ni 1/3 Mn 1/3 O 2 as alternative cathode material to commercially used LiCoO 2 in lithium rechargeable battery has been performed. Parameters of a local atomic structure such as radii of metal-oxygen and metal-metal coordination shells and disorder in those shells have been determined. It has been found that the radius of the first coordination shell (metal-oxygen) as well as a local disorder in the second shell (metal-metal) around each of the 3d-metals are in a good agreement with obtained for superlattice model of √3 x √3] R30 o type in triangular lattice of sites by first principle calculation. Other parameters of the local atomic structure around Co, Ni and Mn atoms do not provide evidence for presence of superstructure in LiCo 1/3 Ni 1/3 Mn 1/3 O 2

(1R,2R,3R,4R,5S-2,3-Bis[(2S′-2-acetoxy-2-phenylacetoxy]-4-azido-1-[(2,4-dinitrophenylhydrazonomethyl]bicyclo[3.1.0]hexane

Directory of Open Access Journals (Sweden)

Robert McDonald

2008-02-01

Full Text Available In the title compound, C38H29N7O12, the five-membered ring adopts an envelope conformation in which the `flap' is cis to the cyclopropane group. This conformation is similar to those of other bicyclo[3.1.0]hexane analogues for which crystal structures have been reported. The absolute configuration of the stereogenic centers on the cyclopentane ring, as determined by comparison with the known configurations of the stereogenic centers in the (2S-2-acetoxy-2-phenylacetoxy groups, is 1(R, 2(R, 3(R, 4(R and 5(S. An intramolecular N—H...O hydrogen bond is present.

Electron-impact excitation of multiply-charged ions using energy loss in merged beams: e + Si3+(3s2S1/2) → e + Si3+(3p2P1/2,3/2)

International Nuclear Information System (INIS)

Wahlin, E.K.; Thompson, J.S.; Dunn, G.H.; Phaneuf, R.A.; Gregory, D.C.; Smith, A.C.H.

1990-01-01

For the first time absolute total cross sections for electron-impact excitation of a multiply-charged ion have been measured using an electron-energy-loss technique. Measurements were made near threshold for the process e + Si 3+ (3s 2 S 1/2 ) → e + Si 3+ (3p 2 P 1/2 , 3/2 ) -- 8.88 eV. The 10 -15 cm 2 measured cross section agrees with results of 7-state close coupling calculations to better than the ±20% (90% CL) total uncertainty of the measurements. Convoluting the theoretical curve with a Gaussian energy distribution indicates an energy width of 0.15 approx-lt ΔE approx-lt 0.20 eV. 12 refs., 2 figs

(E-3-Methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone

Directory of Open Access Journals (Sweden)

Yordanka Ivanova

2016-09-01

Full Text Available The title compound, (E-3-methyl-6-(3-oxo-3-(3,4,5-trimethoxyphenylprop-1-en-1-yl-2(3H-benzothiazolone, was synthesized by both an acid- and base-catalyzed aldol condensation of 3-methyl-6-acetyl-2(3H-benzothiazolone and 3,4,5-trimethoxyacetophenone. The structure of the target compound was confirmed using 1H-NMR, 13C-NMR, IR, MS, and elemental analysis.

1-[3-(2-Nitrophenyl-5-phenyl-2-pyrazolin-1-yl]ethanone

Directory of Open Access Journals (Sweden)

Huan-Mei Guo

2010-07-01

Full Text Available The title compound, C17H15N3O3, was prepared from 1-(2-nitrophenyl-3-phenylprop-2-en-1-one and hydrazine. The dihedral angle between the benzene and phenyl rings is 74.55 (2°. The pyrazoline ring is in a slight envelope conformation with the C atom bonded to the phenyl ring forming the flap. In the crystal structure, weak intermolecular C—H...O hydrogen bonds connect molecules into chains along [100].

Multiple anion...π interactions in tris(1,10-phenanthroline-κ(2)N,N')iron(II) bis[1,1,3,3-tetracyano-2-(2-hydroxyethyl)propenide] monohydrate.

Science.gov (United States)

Setifi, Zouaoui; Domasevitch, Konstantin V; Setifi, Fatima; Mach, Pavel; Ng, Seik Weng; Petříček, Vaclav; Dušek, Michal

2013-11-01

In the ionic structure of the title compound, [Fe(C12H8N2)3](C9H5N4O2)2·H2O, the octahedral tris-chelate [Fe(phen)3](2+) dications [Fe-N = 1.9647 (14)-1.9769 (14) Å; phen is 1,10-phenathroline] afford one-dimensional chains by a series of slipped π-π stacking interactions [centroid-to-centroid distances = 3.792 (3) and 3.939 (3) Å]. The 1,1,3,3-tetracyano-2-(2-hydroxyethyl)propenide anions, denoted tcnoetOH(-), reveal an appreciable delocalization of π-electron density, involving the central propenide [C-C = 1.383 (3)-1.401 (2) Å] fragment and four nitrile groups, and this is also supported by density functional theory (DFT) calculations at the B97D/6-311+G(2d,2p) level. Primary noncovalent inter-moiety interactions comprise conventional O-H...O(N) and weak C-H...O(N) hydrogen bonding [O...O(N) = 2.833 (2)-3.289 (5) Å and C...O(N) = 3.132 (2)-3.439 (2) Å]. The double anion...π interaction involving a nitrile group of tcnoetOH(-) and two cis-positioned pyridine rings (`π-pocket') of [Fe(phen)3](2+) [N...centroid = 3.212 (2) and 3.418 (2) Å] suggest the relevance of anion...π stackings for charge-diffuse polycyanoanions and common M-chelate species.

Human safety and pharmacokinetics of the CFC alternative propellants HFC 134a (1,1,1,2-tetrafluoroethane) and HFC 227 (1,1,1,2,3,3,3-heptafluoropropane) following whole-body exposure

NARCIS (Netherlands)

Emmen, H.H.; Hoogendijk, E.M.G.; Klöpping-Ketelaars, W.A.A.; Muijser, H.; Duistermaat, E.; Ravensberg, J.C.; Alexander, D.J.; Borkhataria, D.; Rusch, G.M.; Schmit, B.

2000-01-01

HFC 134a (1,1,1,2-tetrafluoroethane) and HFC 227 (1,1,1,2,3,3,3-heptafluoropropane) are used to replace chlorofluorocarbons (CFCs) in refrigerant and aerosol applications, including medical use in metered-dose inhalers. Production and consumption of CFCs are being phased out under the Montreal

HANSF 1.3.2 User's Manual

International Nuclear Information System (INIS)

DUNCAN, D.R.

1999-01-01

The HANSF analysis tool is an integrated model considering phenomena inside a multi-canister overpack (MCO) spent nuclear fuel container such as fuel oxidation, convective and radiative heat transfer, and the potential for fission product release. This manual reflects the HANSF version 1.3.2, a revised version of 1.3.1. HANSF 1.3.2 was written to correct minor errors and to allow modeling of condensate flow on the MCO inner surface. HANSF 1.3.2 is intended for use on personal computers such as IBM-compatible machines with Intel processors running under Lahey TI or digital Visual FORTRAN, Version 6.0, but this does not preclude operation in other environments

Fragrance material review on 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one.

Science.gov (United States)

Scognamiglio, J; Letizia, C S; Api, A M

2013-12-01

A toxicologic and dermatologic review of 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one when used as a fragrance ingredient is presented. 3-Methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)pent-3-en-2-one were evaluated then summarized and includes physical properties, acute toxicity, skin irritation, mucous membrane (eye) irritation, sensitization, phototoxicity, photoallergy, and genotoxicity data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones when used as fragrance ingredients. Submitted for publication) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

Note: High-power piezoelectric transformer fabricated with ternary relaxor ferroelectric Pb(Mg(1/3)Nb(2/3))O3-Pb(In(1/2)Nb(1/2))O3-PbTiO3 single crystal.

Science.gov (United States)

Wang, Qing; Ma, Chuanguo; Wang, Feifei; Liu, Bao; Chen, Jianwei; Luo, Haosu; Wang, Tao; Shi, Wangzhou

2016-03-01

A plate-shaped piezoelectric transformer was designed and fabricated using ternary relaxor ferroelectric single crystal Pb(Mg(1/3)Nb(2/3))O3-Pb(In(1/2)Nb(1/2))O3-PbTiO3. Both the input and output sections utilized the transverse-extensional vibration mode. The frequency and load dependences of the electrical properties for the proposed transformer were systematically studied. Results indicated that under a matching load resistance of 14.9 kΩ, a maximum output power of 2.56 W was obtained with the temperature rise less than 5 °C. The corresponding power density reached up to 50 W/cm(3). This ternary single-crystal transformer had potential applications in compact-size converters requiring high power density.

Synthesis of (+-)-[1,1'-15N2, 2'-13C]-trans-3'-methylnicotine

International Nuclear Information System (INIS)

Sirimanne, S.R.; Maggio, V.L.; Patterson, D.G. Jr.

1992-01-01

The synthesis of (±)- [1,1'- 15 N 2 , 2'- 13 C]-trans-3'-methylnicotine is reported. 15 N-3-Bromopyridine obtained from bromination of pyridine was formylated with nBuLi/[carbonyl- 13 C]-methyl formate. The resulting 15 n-Pyridine-3-[ 13 C-carbonyl]-carboxaldehyde was reacted with 15 N-methylamine and then the resulting Schiff's base was condensed with succinic anhydride to give (±)- [1,1'- 15 N 2 , 5'- 13 C]-trans-4'-carboxycotinine. Reduction with lithium aluminum hydride and mesylation followed by reduction with Zn/NaI gave (±)-[1,1'- 15 N 2 , 2'- 13 C]-trans-3'-methylnicotine. (Author)

Preparation of YBa2Cu3O7-δ powders by the thermal decomposition of a heteronuclear complex, CuY1/3Ba2/3(dhbaen)(NO3)1/3(H2O)3

International Nuclear Information System (INIS)

Hasegawa, E.; Aono, H.; Sadaoka, Y.; Traversa, E.

1999-01-01

YBa 2 Cu 3 O 7-δ powders were prepared by the thermal decomposition of a heteronuclear complex, CuY 1/3 Ba 2/3 (dhbaen)(NO 3 ) 1/3 (H 2 O) 3 . The products of the complex thermal decomposition were analyzed by TG-DTA, XRD, SEM-Auger and XPS. The decomposition of the CuY 1/3 Ba 2/3 -complex was obtained at about 500 C and the product was a mixture of oxides and carbonates. The formation of YBa 2 Cu 3 O 7-δ proceeded at 800 C, with a gradual decomposition of the carbonates. A homogeneous distribution of each element, Y, Ba, and Cu, was observed for the decomposed CuY 1/3 Ba 2/3 -complex by SEM-Auger analysis. The binding energy values of Ba3d 5/2 and O1s photolines from Ba and O in the superconductive lattice did not shift during the sputtering period. Furthermore, the formation of Ba rich regions on the surface was depressed by using the complex as a starting material for homogeneous 123-oxide, YBa 2 Cu 3 O 7-δ . (orig.)

Stable Sheave Moduli of Rank 2 with Chern Classes c 1 = -1; c2 = 2; c3 = 0 on Q3

Directory of Open Access Journals (Sweden)

A. D. Uvarov

2012-01-01

Full Text Available In this paper we consider the scheme MQ( 2;¡1; 2; 0 of stable torsion free sheaves of rank 2 with Chern classes c1 = -1, c2 = 2, c3 = 0 on a smooth 3-dimensional projective quadric Q. The manifold MQ(-1; 2 of moduli bundles of rank 2 with Chern classes c1 = -1, c2 = 2 on Q was studied by Ottaviani and Szurek in 1994. In 2007 the author described the closure MQ (-1; 2 in the scheme MQ(2;¡1; 2; 0. In this paper we prove that in MQ(2;¡1; 2; 0 there exists a unique irreducible component diferent from MQ (¡1; 2 which is a rational variety of dimension 10.

Neutron investigation of Ru-doped Nd1/2Ca1/2MnO3. Comparison with Cr-doped Nd1/2Ca1/2MnO3

International Nuclear Information System (INIS)

Moritomo, Yutaka; Nonobe, Toshihiko; Machida, Akihiko; Ohoyama, Kenji

2002-01-01

Lattice and magnetic properties are investigated for 3% Ru- and Cr-doped Nd 1/2 Ca 1/2 MnO 3 . The parent Nd 1/2 Ca 1/2 MnO 3 is a charge-ordered insulator (T CO =250K). With decreasing temperature below ≅210K, these compounds are separated into two perovskite phases, that is, the long-c and short-c phases. The long-c region shows a ferromagnetic transition at T C ≅210K for the Ru-doped compound and ≅130K for the Cr-doped compound, while the short-c region shows antiferromagnetic transition at T N ≅150K for Ru and ≅110K for Cr. We discuss the origin of the enhanced T C for the Ru-doped compound in terms of the effective one-electron bandwidth W of the e g -band. (author)

New 4-phosphino-1,3,2-dioxaborinanes

International Nuclear Information System (INIS)

Musina, Eh.I.; Nikonov, G.N.; Balueva, A.S.; Litvinov, I.A.

1999-01-01

Molecular and crystal structure of bis[(5,6-benzo-2-phenyl-1,3,2-dioxaborinane-4)phenylphosphino]methane are ascertained by the method of X-ray diffraction analysis. Interaction of methyl (phenyl) phosphine and salicyl aldehyde with phenylboric acid ester gives rise to preparation of its monoheterocyclic analog - 4-methyl(phenyl) phosphino-2-phenyl-5,6-benzo-1,3,2-dioxaborinane and its sulfide. It is shown that in the series 4-aryl(alkyl)phosphino 1,3,2-dioxaborinanes no stacking-conformations realized for 4-diarylphosphino-1,3,2-dioxaboraphosphorinanes are observed [ru

S-Alkylated/aralkylated 2-(1H-indol-3-yl-methyl)-1,3,4- oxadiazole-5 ...

African Journals Online (AJOL)

ylmethyl)-1,3,4- oxadiazole-5-thiol derivatives. Methods: 2-(1H-indol-3-yl)acetic acid (1) was reacted with absolute ethanol and catalytic amount of sulfuric acid to form ethyl 2-(1H-indol-3-yl)acetate (2) which was transformed to 2-(1H-indol-3- ...

GITT studies on oxide cathode LiNi1/3Co1/3Mn1/3O2 synthesized ...

Indian Academy of Sciences (India)

Li diffusion; LiNi1/3Co1/3Mn1/3O2; lithium ion batteries; layered structure. 1. Introduction ... The coin-type cell CR2012 consisting of a metallic- lithium foil anode ... and the polyvinylidenefluoride (PVDF) binder with a mass ratio of 4:1:1 in NMP ...

(E-3-Propoxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one monohydrate

Directory of Open Access Journals (Sweden)

Burkhon Zh Elmuradov

2010-05-01

Full Text Available The title compound, C15H16N2O2·H2O, was synthesized via the alkylation of 3-hydroxymethylidene-2,3-dihydro-1H-pyrrolo[2,1-b]quinazolin-9-one with n-propyl iodide in the presence of sodium hydroxide. The organic molecule and the water molecule both lie on a crystallographic mirror plane. In the crystal structure, intermolecular O—H...O and O—H...N hydrogen bonds link the components into extended chains along [100].

Effect of 24,25-dihydroxyvitamin D3 on 1,25-dihydroxyvitamin D3 [1,25-(OH)2D3] metabolism in vitamin D-deficient rats infused with 1,25-(OH)2D3

International Nuclear Information System (INIS)

Yamato, H.; Matsumoto, T.; Fukumoto, S.; Ikeda, K.; Ishizuka, S.; Ogata, E.

1989-01-01

Previous studies revealed that administration of 24,25-dihydroxyvitamin D3 [24,25-(OH)2D3] to calcium (Ca)-deficient rats causes a dose-dependent reduction in markedly elevated serum 1,25-(OH)2D3 level. Although the results suggested that the metabolism of 1,25-(OH)2D3 was accelerated by 24,25-(OH)2D3, those experiments could not define whether the enhanced metabolism of 1,25-(OH)2D3 played a role in the reduction in the serum 1,25-(OH)2D3 level. In the present study, in order to address this issue more specifically, serum 1,25-(OH)2D3 was maintained solely by exogenous administration through miniosmotic pumps of 1,25-(OH)2D3 into vitamin D-deficient rats. Thus, by measuring the serum 1,25-(OH)2D3 concentration, the effect of 24,25-(OH)2D3 on the MCR of 1,25-(OH)2D3 could be examined. Administration of 24,25-(OH)2D3 caused a dose-dependent enhancement in the MCR of 1,25-(OH)2D3, and 1 microgram/100 g rat.day 24,25-(OH)2D3, which elevated serum 24,25-(OH)2D3 to 8.6 +/- 1.3 ng/ml, significantly increased MCR and suppressed serum levels of 1,25-(OH)2D3. The effect of 24,25-(OH)2D3 on 1,25-(OH)2D3 metabolism developed with a rapid time course, and the recovery of iv injected [1 beta-3H]1,25-(OH)2D3 in blood was significantly reduced within 1 h. In addition, there was an increase in radioactivity in the water-soluble fraction of serum as well as in urine, suggesting that 1,25-(OH)2D3 is rapidly degraded to a water-soluble metabolite(s). Furthermore, the reduction in serum 1,25-(OH)2D3 was associated with a reduction in both serum and urinary Ca levels. Because the conversion of [3H]24,25-(OH)2D3 to [3H]1,24,25-(OH)2D3 or other metabolites was minimal in these rats, 24,25-(OH)2D3 appears to act without being converted into other metabolites. These results demonstrate that 24,25-(OH)2D3 rapidly stimulates the metabolism of 1,25-(OH)2D3 and reduces its serum level

Synthesis and superstructure of La sub(2/3) (Mg sub(1/2)W sub(1/2))O/sub 3/

Energy Technology Data Exchange (ETDEWEB)

Torii, Y [Government Industrial Research Inst., Nagoya (Japan)

1979-10-01

A new perovskite La sub(2/3)(Mg sub(1/2)W sub(1/2))O/sub 3/ having an orthorhombic multiple-cell was synthesized. The lattice constants were a = 7.8157(5) A, b = 7.8344(6) A and c = 2 x 7.9067(6) A. The superstructure was found to be due to a NaCl-type ordering of B ions as well as an ordering of A-site vacancies.

Preparation of layered oxide Li(Co1/3Ni1/3Mn1/3)O2 via the sol-gel process

Institute of Scientific and Technical Information of China (English)

ZHANG Wen; LIU Hanxing; HU Chen; ZHU Xianjun; LI Yanxi

2008-01-01

To obtain homogenous layered oxide Li(Co1/3Ni1/3Ni1/3Mn1/3)O2 as a lithium insertion positive electrode material,the sol-gel process using citric acid as a chelating agent was applied.The material Li(Co1/3,Ni1/3Mn1/3)O2 was synthesized at different calcination temperatures.XRD experiment indicated that the hyered Li(Co1/3Ni1/3Mn1/3)O2material could he synthesized at a lower temperature of 800℃,and the oxidation state of Co,Ni,and Mn in the cathode confirmed by XPS were +3,+2,and +4,respectively.SEM observations showed that the synthesized material could form homogenous particle morphology with the particle size of about 200nm In spite of different calcination temperatures,the charge-discharge curves of all the samples for the initial cycle were similar,and the cathode synthesized at 900℃ showed a small irreversible capacity loss of 11.24% and a high discharge capacity of 212.2 mAh.g-1 in the voltage range of 2.9-4.6 V.

Calculations of resonances parameters for the ((2s2) 1Se, (2s2p) 1,3P0) and ((3s2) 1Se, (3s3p) 1,3P0) doubly excited states of helium-like ions with Z≤10 using a complex rotation method implemented in Scilab

Science.gov (United States)

Gning, Youssou; Sow, Malick; Traoré, Alassane; Dieng, Matabara; Diakhate, Babacar; Biaye, Mamadi; Wagué, Ahmadou

2015-01-01

In the present work a special computational program Scilab (Scientific Laboratory) in the complex rotation method has been used to calculate resonance parameters of ((2s2) 1Se, (2s2p) 1,3P0) and ((3s2) 1Se, (3s3p) 1,3P0) states of helium-like ions with Z≤10. The purpose of this study required a mathematical development of the Hamiltonian applied to Hylleraas wave function for intrashell states, leading to analytical expressions which are carried out under Scilab computational program. Results are in compliance with recent theoretical calculations.

Quenching of I(2P1/2) by O3 and O(3P).

Science.gov (United States)

Azyazov, Valeriy N; Antonov, Ivan O; Heaven, Michael C

2007-04-26

Oxygen-iodine lasers that utilize electrical or microwave discharges to produce singlet oxygen are currently being developed. The discharge generators differ from conventional chemical singlet oxygen generators in that they produce significant amounts of atomic oxygen. Post-discharge chemistry includes channels that lead to the formation of ozone. Consequently, removal of I(2P1/2) by O atoms and O3 may impact the efficiency of discharge driven iodine lasers. In the present study, we have measured the rate constants for quenching of I(2P1/2) by O(3P) atoms and O3 using pulsed laser photolysis techniques. The rate constant for quenching by O3, (1.8 +/- 0.4) x 10(-12) cm3 s-1, was found to be a factor of 5 smaller than the literature value. The rate constant for quenching by O(3P) was (1.2 +/- 0.2) x 10(-11) cm3 s-1.

Magnetocaloric effect in (La1-xAx)2/3Ba1/3Mn1.05O3-δ

DEFF Research Database (Denmark)

Ancona-Torres, Carlos Eugenio; Menon, Mohan; Bahl, Christian Robert Haffenden

Recently, a large magnetocaloric effect has been reported in La2/3Ba1/3MnO3-δ at about 300 K. In this paper, we investigate the effect of the ion size distribution at the A site on the magnetocaloric effect of this perovskite material. This is accomplished by replacing the lanthanum by Ce, Pr......, and Nd, which allows us to study the effect of both the average size, , and the distribution, σrA, on the magnetic properties of the system. Using magnetization and heat capacity measurements, we determine the important magnetocaloric parameters ΔSM and ΔTad of (La1-xAx)2/3Ba1/3Mn1.05O3-δ powders...

Development of analytical methods for the gas chromatographic determination of 1,2-epoxy-3-butene, 1,2:3,4-diepoxybutane, 3-butene-1,2-diol, 3,4-epoxybutane-1,2-diol and crotonaldehyde from perfusate samples of 1,3-butadiene exposed isolated mouse and rat livers

Energy Technology Data Exchange (ETDEWEB)

Bhowmik, S.; Schuster, A.; Filser, J.G.

2003-07-01

Mutagenicity and carcinogenicity of 1,3-butadiene (BD) highly probably results from epoxide metabolites as 1,2-epoxy-3-butene (EB), 1,2:3,4-diepoxybutane (DEB) and 3,4-epoxybutane-1,2-diol (EBD). A further metabolite crotonaldehyde (CA) has also been discussed to be relevant. So far, in BD exposed rodents only EB and DEB concentrations had been quantified. However, the methods used were either not very sensitive or instrumentally expensive. Therefore, the goal of the present work was to establish simple analytical methods selective and sensitive enough to determine all of these compounds and a further secondary BD intermediate, 3-butene-1,2-diol (B-diol), in BD exposed rodent livers. The once-through perfused liver system was chosen for testing the applicability of the methods to be developed, since it enables BD exposures of this quantitatively most relevant metabolising organ near to the in-vivo situation. All the metabolites were extracted from the aqueous perfusion medium and analysed using a gas chromatograph equipped with a mass selective detector (GC/MS) in the PCI mode. (orig.)

Object Permanence in 3 1/2- and 4 1/2-Month-Old Infants.

Science.gov (United States)

Baillargeon, Renee

1987-01-01

Three experiments test object permanenece in 3 1/2- and 4 1/2-month-old infants, and use an impossible-possible-habituation event format. The 4 1/2-month-olds, and the 3 1/2-month-olds who were fast habituators, look reliably longer at the impossible than at the possible event. Results seriously question Piaget's (1954) claims regarding the age at…

2-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]indane-1,3-dione

Directory of Open Access Journals (Sweden)

Abdullah M. Asiri

2011-02-01

Full Text Available The title compound 2-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-indane-1,3-dione (3 was synthesized in high yield by reaction of 3,5-dimethyl-1-phenyl-pyrazole-4-carbaldehyde and indane-1,3-dione in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H NMR, 13C NMR and GC-MS spectral analysis.

The 1:1 co-crystal of triphenyl(2,3,5,6-tetrafluorobenzylphosphonium bromide and 1,1,2,2-tetrafluoro-1,2-diiodoethane

Directory of Open Access Journals (Sweden)

Gabriella Cavallo

2014-01-01

Full Text Available The title compound, C25H18F4P+·Br−·C2F4I2, is a 1:1 co-crystal of triphenyl(2,3,5,6-tetrafluorobenzylphosphonium (TTPB bromide and 1,1,2,2-tetrafluoro-1,2-diiodoethane (TFDIE. The crystal structure consists of a framework of TTPB cations held together by C—H...Br interactions. In this framework, infinite channels along [100] are filled by TFDIE molecules held together in infinite ribbons by short F...F [2.863 (2–2.901 (2Å] interactions. The structure contains halogen bonds (XB and hydrogen bonds (HB in the bromide coordination sphere. TFDIE functions as a monodentate XB donor as only one I atom is linked to the Br− anion and forms a short and directional interaction [I...Br− 3.1798 (7 Å and C—I...Br− 177.76 (5°]. The coordination sphere of the bromide anion is completed by two short HBs of about 2.8 Å (for H...Br with the acidic methylene H atoms and two longer HBs of about 3.0 Å with H atoms of the phenyl rings. Surprisingly neither the second iodine atom of TFDIE nor the H atom on the tetrafluorophenyl group make any short contacts.

2-([1,2,4]triazolo[1,5-c]quinazolin-2-yl-alkyl-(alkaryl-, aryl--amines and their derivatives. (3Н-quinazolin-4-ylidenhydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-ylalkyl-(alkaryl-, aryl-carboxylic acids: features of synthesis, modification and ant

Directory of Open Access Journals (Sweden)

Yu. V. Martynenko

2016-08-01

Full Text Available The combination of different «pharmacophore» components in one structure connected via «linker» functional groups is one of the major and justified approaches for the synthesis of new biologically active substances. In this area (3Н-quinazoline-4-ylidenhydrazides (1,3-dioxo-1,3-dihydro-2H-іsoindol-2-yl-alkyl-(aralkyl-, aryl-carboxylic acids are the most interesting compounds. They contain quinazoline and іsoindole fragments united through аlkyl, аlkaryl and аryl groups and furthermore can be used for the synthesis of new heterocycles. Aim: The purpose of this work is to find antimicrobial and antifungal agents among (3H-quinazolin-4-ylidenehydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl-alkyl-(alkaryl-, aryl-carboxylic acids and their fused derivatives and to establish physical-chemical properties of these compounds and to correlate «structure – activity relationship» for structure optimization. Methods and results. The study of microbiological activity was conducted by disco-diffusion method on Mueller-Hinton agar on the following strains of microorganisms: gram-positive cocci (Staphylococcus aureus ATCC 25923, Enterococcus aeruginosa, E. faecalis ATCC 29212, gram-negative bacteria (Pseudomonas aeruginosa PSS27853, Escherichia coli ATCC 25922, facultative anaerobic gram-negative bacteria (Klebsiella pneumoniaе and fungi (Candida albicans ATCC 885653. Conclusion. The protected aminoacids were used to synthesize unknown (3H-quinazolin-4-ylidenehydrazides (1,3-dioxo-1,3-dihydroisoindolo-2-yl-alkyl-(alkaryl-, aryl-carboxylic acids in the reactions of nucleophilic substitution for the first time. While new [1,2,4]triazolo[1,5-c]quinazolin-2-yl-alkyl-(alkaryl-, aryl-- isoindol-1,3(2H-diones were received by heterocyclization of the last. Structure and identity have been confirmed by elemental analysis, physical and chemical methods (1H NMR spectroscopy, mass-spectrometry. Analysis of the results of microbiological study shows, that

Beam-Mode Piezoelectric Properties of Ternary Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 Single Crystals for Medical Linear Array Applications

Science.gov (United States)

Wang, Wei; Wang, Sheng; Zhang, Yaoyao; Zhao, Xiangyong; Luo, Haosu

2011-11-01

In this work, the dielectric and beam-mode piezoelectric properties of ternary 0.35Pb(In1/2Nb1/2)O3-0.35Pb(Mg1/3Nb2/3)O3-0.30PbTiO3 (PIMNT35/35/30) piezoelectric single crystals were investigated. The Curie temperature ( T C) and rhombohedral-to-tetragonal phase-transition temperature ( T rt) are 187°C and 127°C, about 30°C higher than those of PMNT crystals. The beam-mode coupling coefficient k {33/ w } was found to be 90.3%. Furthermore, 3.5-MHz linear arrays based on PIMNT35/35/30 crystals and Pb(Zr1- x Ti x )O3 ceramic (PZT-5H) were simulated using PiezoCAD software. The results indicate that the sensitivity and -6 dB bandwidth of a PIMNT35/35/30 transducer would be approximately 4 dB and 20% higher, respectively, compared with a traditional PZT transducer.

Optical evidences for an intermediate phase in relaxor ferroelectric Pb(In1/2Nb1/2O3-Pb(Mg1/3Nb2/3O3-PbTiO3 single crystals

Directory of Open Access Journals (Sweden)

Xiaolong Zhang

2016-02-01

Full Text Available The mechanism of low-temperature structural transformation and evolution of polar nano-structures in relaxor ferroelectric Pb(In1/2Nb1/2O3-Pb(Mg1/3Nb2/3O3-xPbTiO3 (x = 0.33, 0.35, and 0.42 single crystals have been investigated with the aid of temperature dependent low-wavenumber Raman scattering (LWRS and photoluminescence (PL spectra. The E(TO1 phonon mode reveals the characteristic relaxational polarization fluctuations associated with the reorientation of either polar nano-regions or polar nano-domains. It was found that these mechanisms are not independent and they can be ascribed to the phonon localization. In addition, a short-range monoclinic phase (Mc can be found below 250 K in the tetragonal phase region by LWRS, which is always associated with the morphotropic phase boundary (MPB and excellent electromechanical properties. It is interesting that PL spectra confirm these results. The present work indicates that external field modulation and change of composition can result in the monoclinic phase and co-existence of multi-phase.

Radiosynthesis and biological evaluation of "1"2"3 I(±)trans-2-hydroxy-5-((E)-3-(iodo)allyloxy)-3-(4-phenyl-1-piperazinyl) tetralin

International Nuclear Information System (INIS)

Assaad, T.; Alrayyes, A.

2013-01-01

This work reports both the radiolabeling and preliminary biodistribution results in rats brain of (±)-["1"2"3 I]-II. The novel benzovesamicol derivative (±)-["1"2"3 I]-II was successfully labeled with iodine-"1"2"3 from its corresponding n-tributyltin, with radiochemical purity greater than 97% and radiochemical yield in the range 50 - 55%. (±)-["1"2"3 I]- II showed a higher accumulation in striatum than in the other regions studied. To determine if (±)-["1"2"3 I]-II could provide an advantage compared to reference compound ["1"2"5 I]-IBVM, a kinetic study was carried out, at each point of the kinetic study, (±)-["1"2"3 I]-II showed a lower specific binding compared to ["1"2"5 I]-IBVM. Time activity curves of (±)-["1"2"3 I]-II confirmed that this compound inferior to ["1"2"5 I]-IBVM to explore the VAChT in vivo by SPECT. Moreover, it is well known that interaction at the VAChT binding site is enantioselective, and therefore, working with enantiomerically pure compounds, could improve the compound activity.(author)

Bis[2-(1,3-benzothiazol-2-ylphenyl-κ2C1,N][1,3-bis(4-bromophenylpropane-1,3-dionato-κ2O,O′]iridium(III

Directory of Open Access Journals (Sweden)

Sung Kwon Kang

2013-08-01

Full Text Available The title complex, [Ir(C15H9Br2O2(C13H8NS2], lies about a crystallographic twofold rotation axis passing through the IrIII atom and the central C atom of the bis(bromophenylpropane-1,3-dionate ligand. The IrIII atom adopts a distorted octahedral geometry coordinated by two N atoms in the axial positions, and two C and two O atoms in the equatorial plane. The dihedral angle between the two thiazole ring systems in the complex is 77.45 (10°.

Stereoisomerism and muscarinic receptor agonists: Synthesis and effects of the stereoisomers of 3-[5-(3-amino-1,2,4-oxadizol)yl]-1-azabicyclo[2.2.1]heptane

NARCIS (Netherlands)

Pombo-Villar, E.; Wiederhold, K.-H.; Mengod, G.; Palacios, J.M.; Supavilai, P.; Boddeke, H.W.G.M.

1992-01-01

The preparation and the biological activities of the four stereoisomers of 3-[5-(3-amino-1,2,5-oxadiazol)yl]-1-azabicyclo [2.2.1]heptane are described. The most potent stereoisomer, 3a, has the 3R,4R configuration, and in vitro activities in (pD2(% efficacy): ileum 8.8 (87%), hippocampus 9.8 (116%)

STEREOISOMERISM AND MUSCARINIC RECEPTOR AGONISTS - SYNTHESIS AND EFFECTS OF THE STEREOISOMERS OF 3-[5-(3-AMINO-1,2,4-OXADIAZOL)YL]-1-AZABICYCLO[2.2.1]HEPTANE

NARCIS (Netherlands)

POMBOVILLAR, E; WIEDERHOLD, KH; MENGOD, G; PALACIOS, JM; SUPAVILAI, P; BODDEKE, HWGM

1992-01-01

The preparation and the biological activities of the four stereoisomers of 3-[5-(3-amino-1,2,4-oxadiazol)yl]-1-azabicyclo [2.2.1]heptane are described. The most potent stereoisomer, 3a, has the 3R,4R configuration, and in vitro activities in (pD2(% efficacy): ileum 8.8 (87%), hippocampus 9.8 (116%)

Synthesis, spectral and antimicrobial activity of [3-(4-chloro-phenoxy-2,4-diisopropyl-2,3,4,5-tetrahydro-1H-3l5-benzo[e][1,3,2]diazaphosphepin-3-ylidene]-alkyl-amine

Directory of Open Access Journals (Sweden)

R. Usha Nagalakshmi

2009-11-01

Full Text Available 3-(4-chlorophenoxy-2,4-diisopropyl-2,3,4,5-tetrahydro-1H-benzo[e][1,3,2]diaza-phosphepine was synthesized starting from 1,2-bis(bromomethylbenzene by reacting with 2 equimolar isopropyl amine, one equimolar PBr3 and then one equimolar 4-chlorophenol, respectively. The Staudinger reaction of the diazaphphosphine with a series of alkyl azides gave the corresponding iminophosphoranes. Antibacterial activities of the synthesized iminophosphoranes were screened

2:1 Charge disproportionation in perovskite-structure oxide La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+}

Energy Technology Data Exchange (ETDEWEB)

Guo, Haichuan; Hosaka, Yoshiteru; Seki, Hayato; Saito, Takashi; Ichikawa, Noriya [Institute for Chemical Research, Kyoto University, Uji, Kyoto 611-0011 (Japan); Shimakawa, Yuichi, E-mail: shimak@scl.kyoto-u.ac.jp [Institute for Chemical Research, Kyoto University, Uji, Kyoto 611-0011 (Japan); Integrated Research Consortium on Chemical Sciences, Uji, Kyoto 611-0011 (Japan)

2017-02-15

La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+} was synthesized at a high pressure and high temperature. The compound crystallizes in a √2a×2a×√2a perovskite cell in which the La and Ca ions at the A site are disordered. At 217 K the Fe{sup 3.67+} shows charge disproportionation to Fe{sup 3+} and Fe{sup 5+} in a ratio of 2:1, and this disproportionation is accompanied by transitions in magnetic and transport properties. The charge-disproportionated Fe{sup 3+} and Fe{sup 5+} are arranged along the <111> direction of the cubic perovskite cell. The local electronic and magnetic environments of Fe in La{sub 1/3}Ca{sub 2/3}FeO{sub 3} are quite similar to those of Fe in La{sub 1/3}Sr{sub 2/3}FeO{sub 3}, and the 2:1 charge disproportionation pattern of Fe{sup 3+} and Fe{sup 5+} in La{sub 1/3}Ca{sub 2/3}FeO{sub 3} is also the same as that in La{sub 1/3}Sr{sub 2/3}FeO{sub 3}. - Graphical abstract: The perovskite-structure oxide La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+} shows charge disproportionation to Fe{sup 3+} and Fe{sup 5+} in a ratio of 2:1, and the charge-disproportionated Fe{sup 3+} and Fe{sup 5+} are arranged along the <111> direction of the cubic perovskite cell. - Highlights: • La{sub 1/3}Ca{sub 2/3}FeO{sub 3} with unusually-high-valence Fe{sup 3.67+} was synthesized at a high pressure and high temperature. • At 217 K the Fe{sup 3.67+} shows charge disproportionation (CD) to Fe{sup 3+} and Fe{sup 5+} in a ratio of 2:1. • The charge-disproportionated Fe{sup 3+} and Fe{sup 5+} are arranged along the <111> direction of the cubic perovskite cell. • The disproportionation is accompanied by transitions in magnetic and transport properties.

Synthesis of 0.3Li2MnO3·0.7LiNi1/3Co1/3Mn1/3O2 cathode materials using 3-D urchin-like MnO2 as precursor for high performance lithium ion battery

International Nuclear Information System (INIS)

Zhao, Chenhao; Hu, Zhibiao; Zhou, Yunlong; Fang, Shuzhen; Cai, Shaohan

2015-01-01

In the paper, we report synthesis of lithium rich layered oxide 0.3Li 2 MnO 3 ·0.7LiNi 1/3 Co 1/3 Mn 1/3 O 2 by using an urchin-like MnO 2 as precursor. The influences of calcination temperatures on the structures and electrochemical performances of as-prepared materials are systematically studied. The results show that the obtained sample can partially retain the morphology of urchin-like precursor especially at low temperature, and a higher calcination temperature helps to improve the layered structure and particle size. As lithium ion battery cathodes, the 750 °C sample with the size of 100–200 nm reveals an optimal electrochemical performance. The initial discharge capacity of 234.6 mAh g −1 with high Coulombic efficiency of 84.6 % can be reached at 0.1C within 2.0–4.7 V. After 50 cycles, the capacity retention can reach 90.2 % at 0.5C. Even at high current density of 5C, the sample also shows a stable discharge capacity of 120.5 mAh g −1 . Anyways, the urchin-like MnO 2 directed route is suitable to prepare 0.3Li 2 MnO 3 ·0.7LiNi 1/3 Co 1/3 Mn 1/3 O 2 as lithium ion battery cathode

2-(1,3-Dithiolan-2-ylidene)-5-(1,3-dithian-2-ylidene)-1,3,4,6- tetrathiapentalene(DHDA-TTP), a hybrid of BDH-TTP and BDA-TTP, and its metallic cation-radical salts.

Science.gov (United States)

Yamada, Jun-ichi; Watanabe, Maki; Toita, Takashi; Akutsu, Hiroki; Nakatsuji, Shin'ichi; Nishikawa, Hiroyuki; Ikemoto, Isao; Kikuchi, Koichi

2002-05-21

The synthesis and electrochemical properties of the DHDA-TTP donor, a hybrid of 2,5-bis(1,3-dithiolan-2-ylidene)-1,3,4,6-tetrathiapentalene (BDH-TTP) and 2,5-bis(1,3-dithian-2-ylidene)-1,3,4,6-tetrathiapentalene (BDA-TTP), has been investigated, and its ability to form metallic cation-radical salts is elucidated.

1-(3-Bromopropylindoline-2,3-dione

Directory of Open Access Journals (Sweden)

Fatima Zahrae Qachchachi

2016-04-01

Full Text Available In the title compound, C11H10BrNO2, the indoline ring system has an r.m.s. deviation of 0.026 Å. The side chain (including the Br atom has a trans–gauche conformation, as indicated by the N—C—C—C and C—C—C—Br torsion angles of −177.5 (3 and 68.1 (3°, respectively. In the crystal, molecules are linked by weak C—H...O hydrogen bonds, forming a three-dimensional network.

Enrichment of variations in KIR3DL1/S1 and KIR2DL2/L3 among H1N1/09 ICU patients: an exploratory study.

Directory of Open Access Journals (Sweden)

David La

Full Text Available BACKGROUND: Infection by the pandemic influenza A (H1N1/09 virus resulted in significant pathology among specific ethnic groups worldwide. Natural Killer (NK cells are important in early innate immune responses to viral infections. Activation of NK cells, in part, depend on killer-cell immunoglobulin-like receptors (KIR and HLA class I ligand interactions. To study factors involved in NK cell dysfunction in overactive immune responses to H1N1 infection, KIR3DL1/S1 and KIR2DL2/L3 allotypes and cognate HLA ligands of H1N1/09 intensive-care unit (ICU patients were determined. METHODOLOGY AND FINDINGS: KIR3DL1/S1, KIR2DL2/L3, and HLA -B and -C of 51 H1N1/09 ICU patients and 105 H1N1-negative subjects (St. Theresa Point, Manitoba were characterized. We detected an increase of 3DL1 ligand-negative pairs (3DL1/S1(+ Bw6(+ Bw4(-, and a lack of 2DL1 HLA-C2 ligands, among ICU patients. They were also significantly enriched for 2DL2/L3 ligand-positive pairs (PVA, P=0.024, Pc=0.047; Odds Ratio:2.563, CI95%:1.109-5.923, 3DL1*00101 (Ab>VA, PSTh, P=0.034, Pc=0.268, and 3DL1*029 (Ab>STh, P=0.039, Pc=0.301. Aboriginal patients ligand-positive for 3DL1/S1 and 2DL1 had the lowest probabilities of death (R(d (R(d=28%, compared to patients that were 3DL1/S1 ligand-negative (R(d=52% or carried 3DL1*029 (R(d=52%. Relative to Caucasoids (CA, two allotypes were enriched among non-aboriginal ICU patients (NAb: 3DL1*00401 (NAb>CA, P<0.001, Pc<0.001 and 3DL1*01502 (CA3DL1/S1, 2DL2/L3, and 2DL1 had the lowest probabilities of death (R(d=36%, compared to subjects with 3DL1*01502 (R(d=48% and/or 3DL1*00401 (R(d=58%. CONCLUSIONS: Specific KIR3DL1/S1 allotypes, 3DL1/S1 and 2DL1 ligand-negative pairs, and 2DL2/L3 ligand-positive pairs were enriched among ICU patients. This suggests a possible association with NK cell dysfunction in patients with overactive immune responses to H1N1/09, leading to

5-(4-Bromophenyl-2-(3,4-methylenedioxyphenyl-3-methylsulfanyl-1-benzofuran

Directory of Open Access Journals (Sweden)

Hong Dae Choi

2009-10-01

Full Text Available The title compound, C22H15BrO3S, crystallizes with four molecules in the asymmetric unit. The 4-bromophenyl rings are rotated out of the benzofuran planes, with dihedral angles for the four molecules of 20.8 (2, 17.8 (2, 23.5 (4 and 23.9 (4°. The dihedral angles between the 3,4-methylenedioxyphenyl ring and the benzofuran plane are 13.5 (2, 7.1 (2, 18.6 (3 and 14.2 (3° in the four molecules. The crystal structure is stabilized by weak nonclassical intermolecular C—H...O hydrogen bonds. The crystal structure also exhibits intermolecular aromatic π–π interactions between the benzene and furan rings and between the 4-bromophenyl and 3,4-methylenedioxyphenyl rings from molecules of the same type; the centroid–centroid distances are 3.92 (1 and 3.79 (1, 3.91 (1, 3.77 (1 and 3.77 (1, and 3.79 (1 and 3.75 (1Å in the four molecules.

Improved wavelengths for the 1s2s3S1-1s2p3P0,2 transitions in helium-like Si12+

International Nuclear Information System (INIS)

Armour, I.A.; Myers, E.G.; Silver, J.D.; Traebert, E.; Oxford Univ.

1979-01-01

The wavelengths of the 1s2s 3 S 1 -1s2p 3 P 0 , 2 transitions in He-like Si 12+ have been remaesured to be 87.86 +- 0.01 nm and 81.48 +- 0.01 nm. The use of Rydberg lines for the calibration of fast beam spectra is discussed. (orig.)

Processing of water-based LiNi1/3Mn1/3Co1/3O2 pastes for ...

Indian Academy of Sciences (India)

Results show that a substitution of the conventional organic solvent-based manufacturing route for LiNi1/3Mn1/3Co1/3O2 cathodes by water-based processing exhibits a promising way to realise Li-ion batteries with comparable electrochemical behaviour, while avoiding toxic processing aids and reducing overall ...

Crystal structures of 2,3-bis(4-chlorophenyl-1,3-thiazolidin-4-one and trans-2,3-bis(4-chlorophenyl-1,3-thiazolidin-4-one 1-oxide

Directory of Open Access Journals (Sweden)

Hemant P. Yennawar

2015-03-01

Full Text Available In the crystal structures of the title compounds, C15H11Cl2NOS, (1, and C15H11Cl2NO2S, (2, wherein (2 is the oxidized form of (1, the thiazolidine ring is attached to two chlorophenyl rings. The chlorophenyl ring on the 2-carbon atom position points in the same direction as that of the S atom in (1, while in (2, the S atom points in the opposite direction. The O atom on the chiral S atom in (2 is trans to the chlorophenyl ring on the 2-carbon. The chlorophenyl ring planes in each structure are close to orthogonal, making dihedral angles of 78.61 (6 and 87.46 (8° in (1 and (2, respectively. The thiazolidine ring has a twisted conformation on the S—Cmethine bond in (1, and an envelope conformation with the S atom 0.715 (3 Å out of the plane of other four atoms in (2. In the crystal of (1, molecules are linked by C—H...O hydrogen bonds, as well as by slipped parallel π–π interactions [inter-centroid distance = 3.840 (3 Å] between inversion-related phenyl rings, forming sheets parallel to (001. In the crystal of (2, molecules are linked via C—H...O and C—H...Cl hydrogen bonds, forming slabs parallel to (001.

2-Aminopyrimidine-3,3,3-triphenylpropanoic acid (1/1).

Science.gov (United States)

Serafin, Mateusz F; Wheeler, Kraig A

2007-11-01

The title bimolecular compound, C(4)H(5)N(3).C(21)H(18)O(2), constructed from 2-aminopyrimidine and 3,3,3-triphenylpropanoic acid, forms a tetramolecular hydrogen-bonded motif via O-H...N, N-H...O and N-H...N contacts. This aggregate organizes to give crystal-packing motifs with hydrophilic and hydrophobic regions.

1-[3-(2-Methyl-4-phenylquinolin-3-yl-5-phenyl-4,5-dihydro-1H-pyrazol-1-yl]-propane-1-one

Directory of Open Access Journals (Sweden)

Allaoua Kedjadja

2015-06-01

Full Text Available A novel compound, 1-[3-(2-methyl-4-phenylquinolin-3-yl-5-phenyl-4,5-dihydro-1H-pyrazol-1-yl]-propane-1-one (3 has been synthesized by cyclocondensation of (E-1-(2-methyl-4-phenylquinolin-3-yl-3-phenylprop-2-en-1-one (2 and hydrazine hydrate in propionic acid. The structure of this compound was established by elemental analysis, IR, 1H-NMR, 13C-NMR and MS data.

Calculations of resonances parameters for the ((2s2) 1Se, (2s2p) 1,3P0) and ((3s2) 1Se, (3s3p) 1,3P0) doubly excited states of helium-like ions with Z≤10 using a complex rotation method implemented in Scilab

International Nuclear Information System (INIS)

Gning, Youssou; Sow, Malick; Traoré, Alassane; Dieng, Matabara; Diakhate, Babacar; Biaye, Mamadi; Wagué, Ahmadou

2015-01-01

In the present work a special computational program Scilab (Scientific Laboratory) in the complex rotation method has been used to calculate resonance parameters of ((2s 2 ) 1 S e , (2s2p) 1,3 P 0 ) and ((3s 2 ) 1 S e , (3s3p) 1,3 P 0 ) states of helium-like ions with Z≤10. The purpose of this study required a mathematical development of the Hamiltonian applied to Hylleraas wave function for intrashell states, leading to analytical expressions which are carried out under Scilab computational program. Results are in compliance with recent theoretical calculations. - Highlights: • Resonance energy and widths computed for doubly excited states of helium-like ions. • Well-comparable results to the theoretical literature values up to Z=10. • Satisfactory agreements with theoretical calculations for widths

A Comparative Study of the Inclusion Complexes of 2-[5'-benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole and 2-[5'-(p-N,N-dimethylamino- benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole withβ-Cyclodextrin

Directory of Open Access Journals (Sweden)

S. Panda

2011-01-01

Full Text Available The compounds 2-[5'-benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole and 2-[5'-(p-N,N-dimethylamino- benzylidene-2'-phenyl-4'-oxo-1', 3'-thiazolidine]-1, 3-benzothiazole have been synthesized in their purest forms starting from 2-aminobenzothiazole. The inclusion complexes of the above compounds have been prepared with β-cyclodextrin to increase their solubility and bioaccessibility in polar medium. The formation of inclusion complexes have been ascertained by study of spectral characteristic before and after inclusion complex formation. The stability of inclusion complexes and nature of interaction between the host and guest are known from the determination of thermodynamic parameters. Further the antibacterial and antifungal activities of the compounds are determined which is found to increase significantly after inclusion complex formation

2-[1-(1-Naphthyl-1H-1,2,3-triazol-4-yl]pyridine

Directory of Open Access Journals (Sweden)

Ulrich S. Schubert

2009-05-01

Full Text Available In the crystal structure of the title compound, C17H12N4, the angle between the naphthalene and 1H-1,2,3-triazole ring systems is 71.02 (4° and that between the pyridine and triazole rings is 8.30 (9°.

GITT studies on oxide cathode LiNi1/3Co1/3Mn1/3O2 synthesized ...

Indian Academy of Sciences (India)

2016-08-26

Aug 26, 2016 ... GITT studies on oxide cathode LiNi1/3Co1/3Mn1/3O2 synthesized by citric acid assisted high-energy ball milling ... The State Key Laboratory Base of Novel Functional Materials and Preparation Science; The Faculty of Materials Science and Chemical Engineering, Ningbo University, Ningbo 315211, P. R. ...

Layered oxides-LiNi1/3Co1/3Mn1/3O2 as anode electrode for symmetric rechargeable lithium-ion batteries

Science.gov (United States)

Wang, Yuesheng; Feng, Zimin; Yang, Shi-Ze; Gagnon, Catherine; Gariépy, Vincent; Laul, Dharminder; Zhu, Wen; Veillette, René; Trudeau, Michel L.; Guerfi, Abdelbast; Zaghib, Karim

2018-02-01

High-performance and long-cycling rechargeable lithium-ion batteries have been in steadily increasing demand for the past decades. Nevertheless, the two dominant anodes at the moment, graphite and L4T5O12, suffer from a safety issue of lithium plating (operating voltage at ∼ 0.1 V vs. Li+/Li) and low capacity (175 mAh/g), respectively. Here, we report LiNi1/3Co1/3Mn1/3O2 as an alternative anode material which has a working voltage of ∼1.1 V and a capacity as high as 330 mAh/g at the current rate of C/15. Symmetric cells with both electrodes containing LiNi1/3Co1/3Mn1/3O2 can deliver average discharge voltage of 2.2 V. In-situ XRD, HRTEM and first principles calculations indicate that the reaction mechanism of a LiNi1/3Co1/3Mn1/3O2 anode is comprised mainly of conversion. Both the fundamental understanding and practical demonstrations suggest that LiNi1/3Co1/3Mn1/3O2 is a promising negative electrode material for lithium-ion batteries.

1-Ethyl-5-iodoindoline-2,3-dione

Directory of Open Access Journals (Sweden)

Lei Wang

2014-01-01

Full Text Available There are two independent molecules in the asymmetric unit of the title compound, C10H8INO2, which differ in the degree of planarity. The iodoindoline-2,3-dione skeleton of molecule 1 is essentially planar [mean deviation = 0.003 (2 Å for the nine non-H atoms of the indoline core, with a maximum deviation of 0.033 (1 Å for the I atom]. The I atom and O atom in the 3-position of molecule 2 deviate by 0.195 (1 and 0.120 (2 Å, respectively, from the least-squares plane through the nine non-H atoms of the indoline core. Molecules 1 and 2 are roughly coplanar, the mean planes through their cores making a dihedral angle of 6.84 (1°. This coplanarity results in a layer-like structure parallel to (6,11,17 in the crystal, the distance between adjacent least-squares planes through the cores of molecules 1 and 2 being 3.37 (1 Å. In such a layer, molecules 1 and 2 are linked by C—H...O hydrogen bonds, forming chains along [11-1]. The chains are further coupled to construct a kind of double-chain structure via I...O interactions [3.270 (2 Å].

Switchable Synthesis of 4,5-Functionalized 1,2,3-Thiadiazoles and 1,2,3-Triazoles from 2-Cyanothioacetamides under Diazo Group Transfer Conditions.

Science.gov (United States)

Filimonov, Valeriy O; Dianova, Lidia N; Galata, Kristina A; Beryozkina, Tetyana V; Novikov, Mikhail S; Berseneva, Vera S; Eltsov, Oleg S; Lebedev, Albert T; Slepukhin, Pavel A; Bakulev, Vasiliy A

2017-04-21

High yield solvent-base-controlled, transition metal-free synthesis of 4,5-functionalized 1,2,3-thiadiazoles and 1,2,3-triazoles from 2-cyanothioacetamides and sulfonyl azides is described. Under diazo transfer conditions in the presence of a base in an aprotic solvent 2-cyanothioacetamides operating as C-C-S building blocks produce 5-amino-4-cyano-1,2,3-thiadiazoles exclusively. The use of alkoxide/alcohol system completely switches the reaction course due to the change of one of the reaction centers in the 2-cyanothioacetamide (C-C-N building block) resulting in the formation of 5-sulfonamido-1,2,3-triazole-4-carbothioamide sodium salts as the only products. The latter serve as good precursors for 5-amino-1,2,3-thiadiazole-4-carboximidamides, the products of Cornforth-type rearrangement occurring in neutral protic medium or under acid conditions. According to DFT calculations (B3LYP/6-311+G(d,p)) the rearrangement proceeds via intermediate formation of a diazo compound, and can be catalyzed by acids via the protonation of oxygen atom of the sulfonamide group.

Poly[propane-1,3-diammonium [cuprate(II-bis(μ2-pyridine-2,3-dicarboxylato] trihydrate

Directory of Open Access Journals (Sweden)

Shabnam Hooshmand

2008-02-01

Full Text Available The title polymeric compound {(C3H12N2[Cu(C7H3NO42]·3H2O}n or {(pnH2[Cu(py-2,3-dc2]·3H2O}n (pn is propane-1,3-diamine and py-2,3-dcH2 is pyridine-2,3-dicarboxylic acid, was synthesized by reaction of copper(II chloride dihydrate with a proton-transfer compound, propane-1,3-diammonium pyridine-2,3-dicarboxylate or (pnH2(py-2,3-dc, in aqueous solution. The anion is a six-coordinate complex (site symmetry overline{1}, with a distorted octahedral geometry around CuII, consisting of two bidentate pyridine-2,3-dicarboxylate groups and two O atoms of bridging ligands from (py-2,3-dc2− fragments, which are located in trans positions. The (pnH22+ cation is disordered over two sites by the center of inversion. Intermolecular hydrogen bonds, π–π [centroid–centroid distances of 3.539 (3 Å] and C—O...π stacking interactions [O...Cg = 3.240 (5 Å; Cg is the center of the pyridine ring], connect the various components into a supramolecular structure.

1-(1-Hydroxy-9H-carbazol-2-yl-3-methylbut-2-en-1-one

Directory of Open Access Journals (Sweden)

Matthias Zeller

2010-02-01

Full Text Available The title compound, C17H15NO2, was prepared as one of two products of the AlCl3/POCl3-catalysed reaction of 9-carbazol-1-ol with 3,3-dimethyacrylic acid. It crystallizes with two crystallographically independent molecules, A and B, which are virtually superimposable but not related by any translational or other pseudosymmetry. Both independent molecules are almost planar [r.m.s. deviations from planarity = 0.053 (1 and 0.079 (1 Å in A and B, respectively] and contain an intramolecular O—H...O hydrogen bond. Each type of molecules is connected via pairs of N—H...O hydrogen bonds, forming centrosymmetric A2 and B2 dimers which are, in turn, arranged in offset π-stacks extending along the a-axis direction. The offset of the dimers and the tilt angle of the molecules allows the formation of alternating C—H...π interactions between A and B molecules of parallel stacks.

Gadolinium (III) 2-benzoyl-1,1,3,3-tetracyanopropenide diacetate. Synthesis and crystal structure

Energy Technology Data Exchange (ETDEWEB)

Karpov, Sergey V.; Kayukov, Yakov S.; Grigor' ev, Arthur A. [Department of Chemistry and Pharmaceutics, I.N. Ul' yanov Chuvash State University, Cheboksary (Russian Federation); Tafeenko, Victor A. [Department of Chemistry, Lomonosov Moscow State University (Russian Federation)

2018-02-15

2-Acyl-1,1,3,3-tetracyanopropenides (ATCN) is a stable organic salts, containing the carbonyl group in addition to the tetracyanoallyl (TCA) fragment in the anion. TCA anions are known as bridging ligands with variable denticity with potential application in organic electronics and as a ionic liquids components. In this communication we reporting the synthesis and crystal structure of gadolinium(III) 2-benzoyl-1,1,3,3-tetracyanopropenide diacetate - the first lanthanide ATCN. (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

(E-1-(2-Aminophenyl-3-(benzo[d][1,3]dioxol-5-ylprop-2-en-1-one

Directory of Open Access Journals (Sweden)

Rodrigo Abonia

2016-12-01

Full Text Available The title chalcone (E-1-(2-aminophenyl-3-(benzo[d][1,3]dioxol-5-ylprop-2-en-1-one was obtained in 76% yield from a NaOH catalyzed Claisen–Schmidt condensation reaction between o-aminoacetophenone and piperonal. This product will be used as a key precursor for the development of an alternative route for the total synthesis of the alkaloid Graveoline. Single crystals of the title compound suitable for X-ray diffraction were grown via slow evaporation in ethanol at room temperature. A complete crystallographic study was performed in depth to unequivocally confirm its structure. The crystal structure of the title o-aminochalcone, C16H13NO3, shows two molecules per asymmetric unit (Z = 4 and adopts an E configuration about the C=C double bond. In the title compound, the mean plane of the non-H atoms of the central chalcone fragment C—C(O—C—C—C is as follow: [root-mean-square (r.m.s. deviation = 0.0210 Å for A–B and 0.0493 for C–D molecules]. In the crystal, molecules are linked by N–H...O and C–H...O, hydrogen bonds forming S(6, R22(6 and edge-fused R44(24rings along with C(18 chains running parallel to (110.

Synthesis of novel nitroso acetal derivatives via tandem 6π-electrocyclization/ [3+2]-cycloaddition of 1-nitro-2-methyl-1,3 butadiene

OpenAIRE

Esra Koc

2017-01-01

Novel nitroso acetal derivatives (4-methyl-2,3,3a,6-tetrahydroisoxazolo[2,3-b][1,2]oxazine) were synthesized through 6π-electrocyclization/[3+2]-cycloaddition reaction of several dionophiles with 1-nitro-2-methyl-1,3-butadiene. Structures of the synthesized compounds were determined by 1H-NMR, 13C-NMR, IR and GC-MS analyses.

Diaqua-2κ2O-bis(μ-1-oxido-2-naphthoato-1:2κ3O1,O2:O2′;2:3κ3O2:O1,O2′-bis(1-oxido-2-naphthoato-1κ1O2,O2;3κ2O1,O2-hexapyridine-1κ2N,2κ2N,3κ2N-trimanganese(II/III pyridine disolvate dihydrate

Directory of Open Access Journals (Sweden)

Daqi Wang

2008-12-01

Full Text Available The title complex, [Mn3(C11H6O34(C5H5N6(H2O2]·2H2O·2C5H5N, is a trinuclear mixed oxidation state complex of overline1 symmetry. The three Mn atoms are six-coordinated in the shape of distorted octahedra, each coordinated with an O4N2 set of donor atoms, where the ligands exhibit mono- and bidentate modes. However, the coordination of the MnII ion located on the inversion centre involves water molecules at two coordination sites, whereas that of the two symmetry-related MnIII ions involves an O4N2 set of donor atoms orginating from the organic ligands. Intramolecular C—H...π interactions between neighbouring pyridine ligands stabilize this arrangement. A two-dimensional network parallel to (001 is formed by intermolecular O—H...O hydrogen bonds.

2-(1,3-Dioxoisoindolin-2-ylacetic acid–N′-[(E-2-methoxybenzylidene]pyridine-4-carbohydrazide (1/1

Directory of Open Access Journals (Sweden)

Shaaban K. Mohamed

2012-08-01

Full Text Available In the title 1:1 cocrystal, C10H7NO4·C14H13N3O2, molecules are linked by intermolecular C—H...O, N—H...O and O—H...N hydrogen bonds, forming a three-dimensional network. In addition, π–π stacking interactions [with centroid–centroid distances of 3.5723 (19 and 3.6158 (18 Å] are observed.

Crystal structures of (Z-5-[2-(benzo[b]thiophen-2-yl-1-(3,5-dimethoxyphenylethenyl]-1H-tetrazole and (Z-5-[2-(benzo[b]thiophen-3-yl-1-(3,4,5-trimethoxyphenylethenyl]-1H-tetrazole

Directory of Open Access Journals (Sweden)

Narsimha Reddy Penthala

2016-05-01

Full Text Available (Z-5-[2-(Benzo[b]thiophen-2-yl-1-(3,5-dimethoxyphenylethenyl]-1H-tetrazole methanol monosolvate, C19H16N4O2S·CH3OH, (I, was prepared by the reaction of (Z-3-(benzo[b]thiophen-2-yl-2-(3,5-dimethoxyphenylacrylonitrile with tributyltin azide via a [3 + 2]cycloaddition azide condensation reaction. The structurally related compound (Z-5-[2-(benzo[b]thiophen-3-yl-1-(3,4,5-trimethoxyphenylethenyl]-1H-tetrazole, C20H18N4O3S, (II, was prepared by the reaction of (Z-3-(benzo[b]thiophen-3-yl-2-(3,4,5-trimethoxyphenylacrylonitrile with tributyltin azide. Crystals of (I have two molecules in the asymmetric unit (Z′ = 2, whereas crystals of (II have Z′ = 1. The benzothiophene rings in (I and (II are almost planar, with r.m.s deviations from the mean plane of 0.0084 and 0.0037 Å in (I and 0.0084 Å in (II. The tetrazole rings of (I and (II make dihedral angles with the mean planes of the benzothiophene rings of 88.81 (13 and 88.92 (13° in (I, and 60.94 (6° in (II. The dimethoxyphenyl and trimethoxyphenyl rings make dihedral angles with the benzothiophene rings of 23.91 (8 and 24.99 (8° in (I and 84.47 (3° in (II. In both structures, molecules are linked into hydrogen-bonded chains. In (I, these chains involve both tetrazole and methanol, and are parallel to the b axis. In (II, molecules are linked into chains parallel to the a axis by N—H...N hydrogen bonds between adjacent tetrazole rings.

A New Type of Synthesis of 1,2,3-Thiadiazole and 1,2,3-Diazaphosphole Derivatives Via-Hurd-Mori Cyclization

Directory of Open Access Journals (Sweden)

Mona A. Hosny

2012-01-01

Full Text Available We present a short and efficient synthesis of the title compounds starting with cheap and readily available camphor and derivatives of acetophenone. The optimized sequence allows the large-scale preparation of this new type of synthesis in a few steps. New 1,2,3-thiadiazole and 1,2,3-diazaphosphole derivatives 11-20, were prepared from the ketones 1-5 via the corresponding semicarbazones 6-10. The Hurd-Mori and Lalezari methods were used, respectively, for the preparation of these 1,2,3-thiadiazole and 1,2,3-diazaphospholene derivatives. These derivatives exhibit anticancer effect due to their high potential biological activity.

Fragrance material review on 1-(2,4-dimethyl-3-cyclohexenyl)-2,2-dimethylpropan-1-one.

Science.gov (United States)

Scognamiglio, J; Letizia, C S; Api, A M

2013-12-01

A toxicologic and dermatologic review of 1-(2,4-dimethyl-3-cyclohexenyl)-2,2-dimethylpropan-1-one when used as a fragrance ingredient is presented. 1-(2,4-Dimethyl-3-cyclohexenyl)-2,2-dimethylpropan-1-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 1-(2,4-dimethyl-3-cyclohexenyl)-2,2-dimethylpropan-1-one were evaluated then summarized and includes physical properties, acute toxicity, skin irritation, sensitization, and genotoxicity data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones When Used as Fragrance Ingredients (submitted for publication)) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

Ethyl 2-{4-[(1,5-dibenzyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-1,5-benzodiazepin-3-ylmethyl]-1H-1,2,3-triazol-1-yl}acetate

Directory of Open Access Journals (Sweden)

Hind Jabli

2010-01-01

Full Text Available The reaction of 1,5-dibenzyl-3-propargyl-1,5-benzodiazepine-2,4-dione with ethyl azidoacetate in the presence of copper sulfate pentahydrate and sodium ascorbate leads to the formation of the title regioisomer, C30H29N5O4, which features a phenylene ring fused with a seven-membered diazepinyl ring. The latter ring adopts a boat conformation (with the methyltriazolylacetate-bearing C atom as the prow and the fused-ring C atoms as the stern. The benzyl groups connected to the diazepinyl ring jprotrude from the sides; the methyltriazolylacetate substituent occupies an axial position.

1, 2, 3 ... FAIR !

International Nuclear Information System (INIS)

Sturm, C.; Sharkov, B.; Stoecker, H.

2010-01-01

The Facility for Antiproton and Ion Research FAIR at Darmstadt/Germany will provide worldwide unique accelerator and experimental facilities allowing for a large variety of unprecedented forefront research in hadron, nuclear, atomic and plasma physics and applied sciences. The start version of FAIR, the so called Modularized Start Version includes a basic accelerator as well as three experimental modules - 1, 2, 3 FAIR!

2,4,6-Triamino-1,3,5-triazine-1,3-diium aquapentafluoridoaluminate

Directory of Open Access Journals (Sweden)

V. Maisonneuve

2008-04-01

Full Text Available The title compound, (C3H8N6[AlF5(H2O], was obtained by solvothermal synthesis from the reaction of aluminium hydroxide, 1,3,5-triazine-2,4,6-triamine (melamine, aqueous HF and water at 323 K for 48 h. The structure consists of [AlF5(H2O]2− octahedra and diprotonated melaminium cations. Cohesion is ensured by a three-dimensional network of hydrogen bonds.

Pyridinium 5-[(1,3-diethyl-6-hydroxy-4-oxo-2-thioxo-1,2,3,4-tetrahydropyrimidin-5-yl(2-methoxyphenylmethyl]-1,3-diethyl-4,6-dioxo-2-thioxopyrimidin-5-ide

Directory of Open Access Journals (Sweden)

Abdullah Mohamed Asiri

2009-08-01

Full Text Available 1,3-Diethyl-2-thiobarbituric acid reacts with 2-anisaldehyde to form the Michael addition product 2-anisylbis(1,3-diethyl-2-thiobarbitur-5-ylmethanate, which crystallizes as the title pyridinium salt, C5H6N+·C24H29N4O5S2−, when it reacts with the pyridine used to catalyse the reaction. There are two independent ion pairs in the crystal structure. The anion features a methine C atom connected to three six-membered rings; one of the rings carries a hydroxy group, which engages in hydrogen bonding with the carbonyl group belonging to another ring. The monoclinic unit cell emulates an orthorhombic unit cell, and is a twin with a minor twin component of 35%.

Spherical resonator for vapor-phase speed of sound and measurements of 1,1,1,2,2,3,3-heptafluoro-3-methoxypropane (RE347mcc) and trans-1,3,3,3-tetrafluoropropene [R1234ze(E)

International Nuclear Information System (INIS)

Perkins, Richard A.; McLinden, Mark O.

2015-01-01

Highlights: • A spherical acoustic resonator for gas-phase speed of sound over the range T = (265 to 500) K, p < 10 MPa is described. • The sphere diameter was calibrated with argon and measurements on methane and ethane verified the performance of the system. • The sound speed of RE347mcc was measured over the range T = (325 to 500) K, p < 1.6 MPa. • The sound speed of R1234ze(E) was measured over the range T = (280 to 420) K, p < 2.8 MPa. • The average combined, expanded uncertainties for sound speed were 0.035 m · s"−"1 for RE347mcc and 0.064 m · s"−"1 for R1234ze(E). - Abstract: We describe an apparatus to measure the speed of sound of gas samples at temperatures from (265 to 500) K with pressures up to 10 MPa. The speed of sound was determined from the frequency of the three lowest-order radial resonance modes for the gas in a spherical cavity machined from type 321 stainless steel for corrosion resistance. The spherical resonator was contained in an isothermal copper block that was maintained at the temperature of interest by a multilayer thermostat with vacuum insulation. The dimensions of the spherical cavity were characterized as a function of temperature and pressure though calibration measurements with high-purity argon. The performance of the apparatus was demonstrated with measurements of high-purity methane and ethane. Measurements of the sound speed of 1,1,1,2,2,3,3-heptafluoro-3-methoxypropane (RE347mcc) are reported at temperatures from (325 to 500) K with pressures up to 1.6 MPa. Measurements on trans-1,3,3,3-tetrafluoropropene (R1234ze(E)) are reported at temperatures from (280 to 420) K with pressures up to 2.8 MPa. The average relative combined expanded uncertainties of the measured sound speed for RE347mcc and R1234ze(E) are (0.029 and 0.041)%, respectively.

On a directed variation of the 1-2-3 and 1-2 Conjectures

DEFF Research Database (Denmark)

Barme, Emma; Bensmail, Julien; Przybyło, Jakub

2017-01-01

In this paper, we consider the following question, which stands as a directed analogue of the well-known 1-2-3 Conjecture: Given any digraph D with no arc uv verifying d+(u) = d¯(v) = 1, is it possible to weight the arcs of D with weights among ⟨1; 2; 3⟩ so that, for every arc uv of D, the sum of...

Thermochemistry of 1,3-diethylbarbituric and 1,3-diethyl-2-thiobarbituric acids: Experimental and computational study

International Nuclear Information System (INIS)

Notario, Rafael; Roux, María Victoria; Ros, Francisco; Emel’yanenko, Vladimir N.; Zaitsau, Dzmitry H.; Verevkin, Sergey P.

2014-01-01

Highlights: • Enthalpies of formation in condensed phase have been obtained. • Enthalpy of vaporization of 1,3-diethylbarbituric acid has been determined. • Enthalpy of sublimation of 1,3-diethyl-2-thiobarbituric acid has been determined. • Gas-phase enthalpies of formation have been obtained. • Gas-phase enthalpies of formation have been calculated at G3 and G4 levels. - Abstract: This paper reports an experimental and computational thermochemical study on two barbituric acid derivatives, viz. 1,3-diethylbarbituric acid and 1,3-diethyl-2-thiobarbituric acid. Values of standard molar enthalpies of formation in the gas phase at T = 298.15 K have been derived from experiment. Energies of combustion were measured by the static bomb combustion calorimetry in the case of 1,3-diethylbarbituric acid, and the rotating-bomb combustion calorimetry in the case of 1,3-diethyl-2-thiobarbituric acid. From the combustion energies, standard molar enthalpies of formation in the crystalline state at T = 298.15 K were calculated. The enthalpy of vaporization of 1,3-diethylbarbituric acid and enthalpy of sublimation of 1,3-diethyl-2-thiobarbituric acid were determined using the transpiration method. Combining calorimetric and transpiration results, values of −(611.9 ± 2.0) kJ · mol −1 and −(343.8 ± 2.2) kJ · mol −1 for the gas-phase enthalpies of formation at T = 298.15 K of 1,3-diethylbarbituric and 1,3-diethyl-2-thiobarbituric acids, respectively, were derived. Theoretical calculations at the G3 and G4 levels were performed, and a study of the molecular structure of the compounds has been carried out. Calculated enthalpies of formation were in very good agreement with the experimental values

N-{4-[(2E-3-(2H-1,3-Benzodioxol-5-ylprop-2-enoyl]phenyl}quinoline-3-carboxamide

Directory of Open Access Journals (Sweden)

Efrain Polo

2017-10-01

Full Text Available An amide chalconehas been synthesized in a two-step reaction. First, N-(4-acetylphenylquinoline-3-carboxamide 2 was synthesized by the reaction of quinoline-3-carboxylic acid 1 and thionyl chloride (SOCl2, following the addition of 4-aminoacetophenone. Then, a typical Claisen–Schmidtreactionwas made between 2 and piperonal using KOH solution as a catalystin ethanol, under ultrasonic irradiation. The structure of the target compound was established by FTIR (Fourier-transform infrared spectroscopy, HRMS, 1H and 13C-NMR.

Synthesis and physical-chemical properties of 6-(5-(1Н-tetrazole-1-ylmethyl-4-R-1,2,4-triazole-3-ylthiopyridin-3-amines and 6-((5-(1Н-tetrazole-1-ylmethil-4-R-1,2,4-triazole-3-ylthiopyridin-3-yl-(alk,ar,heterylmethanimines

Directory of Open Access Journals (Sweden)

Yu. S. Hulina

2017-02-01

Full Text Available Over the past decade the number of publications, that contain different aspects of chemistry and use of triazoles and tetrazoles have been doubled and continues to grow. Puplications of recent years show that heterocycles with 1,2,3,4-teterazoles and 1,2,4-triazoles are biologically active compounds with a broad spectrum of action. This fact indicates the interest to these compounds as potential objects of modern pharmaceutical market, namely to those compounds which contain both heterocycles. Purpose – synthesis and establishment of physical-chemical properties of 6-(5-(1Н-tetrazole-1-ylmethyl-4-R-1,2,4-triazole-3-ylthiopyridin-3-amines and 6-((5-(1Н-tetrazole-1-ylmethil-4-R-1,2,4-triazole-3-ylthiopyridin-3-yl-(alk,ar,heterylmethanimines. Materials and methods. The melting point has been determined by capillary method. The elemental composition of compounds has been set with the help of elemental analyzer Elementar Vario L cube (CHNS. 1H NMR spectra of obtained compounds has been set with the help of Varian Mercury VX-200, solvent – DMSO-d6, internal standart – Tetramethylsilane. Chromatography-mass spectrometry studies have been conducted on gas-liquid chromatograph Agilent 1260 Infinity HPLC equipped with a mass spectrometer Agilent 6120. 5-(1H-Tetrazole-1-ylmethyl-4-R-1,2,4-triazole-3-thioles were used as starting materials for 6-(5-(1Н-tetrazole-1-ylmethyl-4-R-1,2,4-triazole-3-ylthiopyridin-3-amines. Synthesis of the compounds was carried out in a medium of propyl alcohol in the presence of 5-amino-2-chloropyridine. 6-((5-(1Н-tetrazole-1-ylmethil-4-R-1,2,4-triazole-3-ylthiopyridin-3-yl-(alk,ar,heterylmethanimines were obtained reacting 6-(5-(1Н-tetrazole-1-ylmethyl-4-R-1,2,4-triazole-3-ylthiopyridin-3-amines with the appropriate aldehydes (acetaldehyde, m-anisaldehyde, 2-hydroxybenzaldehyde, 3-fluorobenzaldehyde, 4-fluorobenzaldehyde, 4-diethylaminobenzaldehyd, hydroxynaphthalene in the acetic acid medium. Results. 11 New

Synthesis, SAR and biological evaluation of a novel series of 1-(2-chloroethyl)-1-nitroso-3-(2-(3-oxobenzoelenazol-2(3H)-yl)ethyl) urea: Organoselenium compounds for cancer therapy.

Science.gov (United States)

Ye, S; Zheng, X; Hu, T; Zeng, H

2016-06-30

Thioredoxin reductase 1 (TrxR1) is an important potential anticancer drug target and closely related to both carcinogenesis and cancer progression. Ethaselen (BBSKE), a novel organoselenium compound inhibiting TrxR1 with selective antitumor effect, while its symmetrical structure results in poor solubility. Carmustine (BCNU), a DNA cross-link agent and also a deactivator of TrxR, is with high toxicity and low selectivity which limit its clinical application to some extents. Herein, a novel compound, 1-(2-chloroethyl)-1-nitroso-3-(2-(3-oxobenzoelenazol-2(3H)-yl)ethyl)urea(4a-1), which was designed through the combination of Ethaselen and Carmustine, showed good solubility, good tagetability, low toxicity and excellent antitumor activity by synergism. Using the structure of 4a-1 as a key active scaffold, a series of novel 1-(2-chloroethyl)-1-nitroso-3-(2-(3-oxobenzoelenazol-2(3H)-yl)ethyl)urea was designed, synthesized and evaluated to explore the structure-activity relationships (SARs) of these inhibitors and to improve their antitumor activities. Notably, 1-(2-chloroethyl)-3-(2-(6-fluoro-3-oxobenzoselenazol-2(3H)-yl)ethyl)-1-nitrosourea(4b-1) was found to exhibit more potent antitumor activities comparable to 4a-1 against all the four cancer cell lines, including Mia PaCa-2, PANC-1, RKO, LoVo. These results have highlighted compound 4b-1 as a new potential lead candidate for future development of novel potent broad-spectrum antitumor agents. In addition, a SAR model was established to conduct further structural modification.

2,2,3,3,5,5,6,6-Octa-p-tolyl-1,4-dioxa-2,3,5,6-tetragermacyclohexane dichloromethane disolvate

Directory of Open Access Journals (Sweden)

Monika L. Amadoruge

2009-09-01

Full Text Available The title compound, C56H56Ge4O2·2CH2Cl2 or Tol8Ge4O2·2CH2Cl2 (Tol = p-CH3C6H4, was obtained serendipitously during the attempted synthesis of a branched oligogermane from Tol3GeNMe2 and PhGeH3. The molecule contains an inversion center in the middle of the Ge4O2 ring which is in a chair conformation. The Ge—Ge bond distance is 2.4418 (5 Å and the Ge—O bond distances are 1.790 (2 and 1.785 (2 Å. The torsion angles within the Ge4O2 ring are −56.7 (1 and 56.1 (1° for the Ge—Ge—O—Ge angles and −43.9 (1° for the O—Ge—Ge—O angle.

5-Methylbenzo[d][2,1,3]selenadiazole

Directory of Open Access Journals (Sweden)

Halima Ouahine

2017-02-01

Full Text Available In the crystal of the title compound, C7H6N2Se, the molecules are arranged in rods along the b-axis direction and form dimeric units due to intermolecular Se...N contacts of 2.982 (2 Å. The molecules are further linked by weak π–π stacking interactions between the 2,1,3-selenadiazole and six-membered aromatic rings [centroid–centroid distance = 3.8509 (11 Å and ring slippage = 1.539 (3 Å].

Henry's law constants and infinite dilution activity coefficients of cis-2-butene, dimethylether, chloroethane, and 1,1-difluoroethane in methanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, isobutanol, tert-butanol, 1-pentanol, 2-pentanol, 3-pentanol, 2-methyl-1-butanol, 3-methyl-1-butanol, and 2-methyl-2-butanol

International Nuclear Information System (INIS)

Miyano, Yoshimori; Kobashi, Takahiro; Shinjo, Hiroshi; Kumada, Shinya; Watanabe, Yusuke; Niya, Wataru; Tateishi, Yoko

2006-01-01

Henry's law constants and infinite dilution activity coefficients of cis-2-butene, dimethylether, chloroethane, and 1,1-difluoroethane in methanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, isobutanol, tert-butanol, 1-pentanol, 2-pentanol, 3-pentanol, 2-methyl-1-butanol, 3-methyl-1-butanol, and 2-methyl-2-butanol in the temperature range of 250 K to 330 K were measured by a gas stripping method and partial molar excess enthalpies were calculated from the activity coefficients. A rigorous formula for evaluating the Henry's law constants from the gas stripping measurements was used for the data reduction of these highly volatile mixtures. The uncertainty is about 2% for the Henry's law constants and 3% for the estimated infinite dilution activity coefficients. In the evaluation of the infinite dilution activity coefficients, the nonideality of the solute such as the fugacity coefficient and Poynting correction factor cannot be neglected, especially at higher temperatures. The estimated uncertainty of the infinite dilution activity coefficients includes 1% for nonideality

N-(2-Methylphenyl-1,2-benzoselenazol-3(2H-one

Directory of Open Access Journals (Sweden)

Xu Zhu

2013-10-01

Full Text Available In the title Ebselen [systematic name: (2-phenyl-1,2-benzoisoselenazol-3-(2H-one] analogue, C14H11NOSe, the benzisoselenazolyl moiety (r.m.s. deviation = 0.0209 Å is nearly perpendicular to the N-arenyl ring, making a dihedral angle of 78.15 (11°. In the crystal, molecules are linked by C—H...O and Se...O interactions into chains along the c-axis direction. The Se...O distance [2.733 (3 Å] is longer than that in Ebselen (2.571 (3 Å].

Poly[(μ3-benzene-1,3,5-tricarboxylato-κ3O1:O3:O5(μ2-2-methylimidazolato-κ2N:N′tris(2-methylimidazole-κNdizinc(II

Directory of Open Access Journals (Sweden)

Palanikumar Maniam

2011-06-01

Full Text Available Hydrothermal reaction involving zinc nitrate hexahydrate, trisodium benzene-1,3,5-tricarboxylate (Na3BTC and 2-methylimidazole (2-MeImH yielded the title compound, [Zn2(C9H3O6(C4H5N2(C4H6N23]. In this mixed-ligand metal-organic compound, Zn2+ ions are coordinated by N atoms from 2-MeImH molecules and (2-MeIm− ions, as well as by O atoms from (BTC3− ions. This results in two different distorted tetrahedra, viz. ZnN3O and ZnN2O2. These tetrahedra are interconnected via (BTC3− ions and N:N′-bridging (2-MeIm− ions, thus forming a layered structure in the bc plane. Hydrogen bonds between the O atoms of carboxylate ions and NH groups of 2-MeImH ligands link the layers into a three-dimensional structure.

Bis[μ-1,2-bis(1H-imidazol-1-ylmethylbenzene-κ2N3:N3′]disilver(I 3-carboxylato-4-hydroxybenzenesulfonate methanol solvate trihydrate

Directory of Open Access Journals (Sweden)

Hong-Mei Sun

2009-09-01

Full Text Available In the title compound, [Ag2(C14H14N42](C7H4O6S·CH3OH·3H2O, the complex dication has a binuclear structure in which each AgI ion is two-coordinated in a slightly distorted linear coordination geometry. The two AgI atoms are bridged by two 1,2-bis[(1H-imidazol-1-ylmethyl]benzene (IBI ligands, forming a 22-membered ring. In the dication, π–π interactions are observed between the imidazole rings with centroid–centroid distances of 3.472 (3 and 3.636 (3 Å. In the crystal, the uncoordinated water molecules, anions and methanol solvent molecules are linked into chains along the b axis by O—H...O hydrogen bonds. In addition, π–π interactions are observed between the benzene rings of the IBI ligands, with a centroid–centroid distance of 3.776 (2 Å. The sulfonate group is disordered over two orientations with occupancies of 0.676 (12 and 0.324 (12.

3-[2-(5H-Indolo[2,3-b]quinoxalin-5-ylethyl]-1,3-oxazolidin-2-one

Directory of Open Access Journals (Sweden)

Abdussalam Alsubari

2010-09-01

Full Text Available The title compound, C19H16N4O2, has an almost planar fused N-heterocyclic system (r.m.s. deviation = 0.031 Å and an almost planar five-membered 1,3-oxazolidine ring (r.m.s. deviation = 0.015 Å at the ends of an ethylene chain [N—C—C—N torsion angle = −65.6 (2°]. The ring systems are inclined at 38.1 (1° to one another.

Synthesis and X-ray Structural Studies of a Substituted 2,3,4,5-Tetrahydro-1H-3-benzazonine and a 1,2,3,5-Tetrahydro-4,3-benzoxazonine

Directory of Open Access Journals (Sweden)

Timothy S. Bailey

2014-12-01

Full Text Available Using a common 1-(1-phenylethenyl-1,2,3,4-tetrahydroisoquinoline precursor to the required ylide or N-oxide intermediate, the Stevens [2,3] and analogous Meisenheimer [2,3] sigmatropic rearrangements have been applied to afford concise syntheses of phenyl -substituted representatives of each of the reduced 1H-3-benzazonine and 4,3-benzoxazonine systems, respectively. Single crystal X-ray structure determinations were employed to define the conformational characteristics for each ring type.

Association of 3BP2 with SHP-1 regulates SHP-1-mediated production of TNF-α in RBL-2H3 cells.

Science.gov (United States)

Chihara, Kazuyasu; Nakashima, Kenji; Takeuchi, Kenji; Sada, Kiyonao

2011-12-01

Adaptor protein 3BP2, a c-Abl Src homology 3 (SH3) domain-binding protein, is tyrosine phosphorylated and positively regulates mast cell signal transduction after the aggregation of the high affinity IgE receptor (FcεRI). Overexpression of the Src homology 2 (SH2) domain of 3BP2 results in the dramatic suppression of antigen-induced degranulation in rat basophilic leukemia RBL-2H3 cells. Previously, a linker for activation of T cells (LAT) was identified as one of the 3BP2 SH2 domain-binding protein. In this report, to further understand the functions of 3BP2 in FcεRI-mediated activation of mast cell, we explored the protein that associates with the SH2 domain of 3BP2 and found that SH2 domain-containing phosphatase-1 (SHP-1) inducibly interacts with the SH2 domain of 3BP2 after the aggregation of FcεRI. The phosphorylation of Tyr(564) in the carboxy (C)-terminal tail region of SHP-1 is required for the direct interaction of SHP-1 to the SH2 domain of 3BP2. The expression of the mutant form of SHP-1 which was unable to interact with 3BP2 resulted in the significant reduction in SHP-1-mediated tumor necrosis factor-α (TNF-α) production without any effects on the degranulation in antigen-stimulated RBL-2H3 cells. These findings suggest that 3BP2 directly interacts with Tyr(564) -phosphorylated form of SHP-1 and positively regulates the function of SHP-1 in FcεRI-mediated signaling in mast cells. © 2011 The Authors. Journal compilation © 2011 by the Molecular Biology Society of Japan/Blackwell Publishing Ltd.

Composites Li2MnO3·LiMn1/3Ni1/3Co1/3O2: Optimized synthesis and applications as advanced high-voltage cathode for batteries working at elevated temperatures

International Nuclear Information System (INIS)

Yu Chuang; Li Guangshe; Guan Xiangfeng; Zheng Jing; Li Liping; Chen Tianwen

2012-01-01

Highlights: ► Composites xLi 2 MnO 3 ·(1 − x)LiMn 1/3 Ni 1/3 Co 1/3 O 2 (x = 0.1–0.4) were prepared by a novel two-step molten-salt route. ► Structure and chemical compositions of the composites were optimized to show an optimum electrochemical property. ► Composite electrode 0.3Li 2 MnO 3 ·0.7LiMn 1/3 Ni 1/3 Co 1/3 O 2 exhibited an excellent electrochemical performance at elevated temperature of 45.4 °C. ► Electrode kinetics of composites was uncovered for the excellent electrochemical performance at elevated temperature. - Abstract: This work reports on the optimized preparation of a series of composites xLi 2 MnO 3 ·(1 − x)LiMn 1/3 Ni 1/3 Co 1/3 O 2 (x = 0.1–0.4) with an aim to find an advanced high-voltage cathode for lithium-ion batteries that can work at elevated temperatures. Developing a two-step molten-salt method leads to composites with a layered-type structure, showing a particle size distribution ranging from 350 to 450 nm. The composites are featured by oxidation states stabilized as Mn 4+ , Ni 2+ , and Co 3+ , and by lattice occupation of Li + in both transition-metal layers and lithium layer of LiMn 1/3 Ni 1/3 Co 1/3 O 2 . When acting as a cathode of lithium-ion batteries, the composite at x = 0.3 shows an optimum electrochemical performance as characterized by a discharge capacity of 120 mAh g −1 at a high current density of 500 mA g −1 and a capacity retention of 64% after 20 cycles. Surprisingly, this electrochemical performance is significantly improved at elevated temperatures. Namely, discharge capacity is increased to 140.4 mAh g −1 at a high current density of 500 mA g −1 , while average capacity decay rate becomes very small to 0.76%. These excellent performance is explained in terms of the dramatically improved lithium-ion diffusions in both electrode and surface films at elevated temperatures.

2-(5-Fluoro-3-isopropylsulfanyl-1-benzofuran-2-ylacetic acid

Directory of Open Access Journals (Sweden)

Pil Ja Seo

2011-11-01

Full Text Available The title compound, C13H13FO3S, was prepared by alkaline hydrolysis of ethyl 2-(5-fluoro-3-isopropylsulfanyl-1-benzofuran-2-ylacetate. In the crystal, the carboxy groups are involved in intermolecular O—H...O hydrogen bonds, which link the molecules into centrosymmetric dimers. These dimers are further packed into stacks along the b axis by a slipped π–π interaction between the furan and benzene rings of neighbouring molecules [centroid–centroid distance = 3.727 (2 Å, interplanar distance = 3.465 (2 Å and slippage = 1.373 (2 Å]. The crystal structure also exhibits a short S...O contact [S...O = 3.219 (2 Å].

Recent Syntheses of 1,2,3,4-Tetrahydroquinolines, 2,3-Dihydro-4(1H-quinolinones and 4(1H-Quinolinones using Domino Reactions

Directory of Open Access Journals (Sweden)

Baskar Nammalwar

2013-12-01

Full Text Available A review of the recent literature is given focusing on synthetic approaches to 1,2,3,4-tetrahydroquinolines, 2,3-dihydro-4(1H-quinolinones and 4(1H-quinolinones using domino reactions. These syntheses involve: (1 reduction or oxidation followed by cyclization; (2 SNAr-terminated sequences; (3 acid-catalyzed ring closures or rearrangements; (4 high temperature cyclizations and (5 metal-promoted processes as well as several less thoroughly studied reactions. Each domino method is presented with a brief discussion of mechanism, scope, yields, simplicity and potential utility.

Dissociative adsorption of CCl 4 on the Fe 3O 4(1 1 1)-(2×2) selvedge of α-Fe 2O 3(0 0 0 1)

Science.gov (United States)

Adib, K.; Mullins, D. R.; Totir, G.; Camillone, N.; Fitts, J. P.; Rim, K. T.; Flynn, G. W.; Osgood, R. M.

2003-02-01

The surface reactions of CCl 4 with the Fe 3O 4(1 1 1)-(2×2) selvedge of naturally occurring α-Fe 2O 3(0 0 0 1) single-crystals have been investigated using synchrotron X-ray photoelectron spectroscopy (XPS) and temperature-programmed desorption (TPD). CCl 4 was found to dissociate on the Fe 3O 4 surface at 100 K producing chemisorbed Cl and adsorbed CCl 2. TPD shows that the large majority of the dissociatively adsorbed CCl 2 fragments extract lattice oxygen and desorb as phosgene at >275 K. However, the XPS spectra show no evidence for the formation of surface-bound phosgene, at 100 K, indicating that its formation involves two steps. The first step, dissociation, is spontaneous at 100 K, whereas the second, oxygen atom abstraction to form phosgene, requires thermal excitation. Cl chemisorption yielded two separate species, the mono- and dichloride terminations of surface iron sites. The identification of these two surface terminations is based on the coverage dependence and the surface temperature history of their Cl 2p 3/2 peak intensity. For example, heating to >450 K allows the monochloride to transform into iron dichloride, indicating Cl adatom mobility at these temperatures.

Structure refinement, far infrared spectroscopy, and dielectric characterization of (1-x)La(Mg1/2Ti1/2)O3-xLa2/3TiO3 solid solutions

Science.gov (United States)

Salak, Andrei N.; Khalyavin, Dmitry D.; Ferreira, Victor M.; Ribeiro, José L.; Vieira, Luís G.

2006-05-01

Dielectric properties of (1-x)La(Mg1/2Ti1/2)O3-xLa2/3TiO3 [(1-x)LMT-xLT] ceramics (0infrared (FIR) frequency ranges. The crystal structure sequence in (1-x)LMT-xLT reported by different authors has been analyzed and revised. FIR spectroscopy was used to characterize the lattice contribution to the dielectric response at microwave frequencies. The complex dielectric function was evaluated from the reflectivity data and extrapolated down to a gigahertz range. Compositional variations of the fundamental microwave dielectric parameters estimated by different methods are compared and discussed. The dependence of the quality factor on the composition in LMT-LT is interpreted in terms of the reduction of spatial phonon correlations originated from the increasing amount of La vacancies. This approach could account for the compositional behavior of the dielectric loss commonly observed in a number of microwave mixed systems.

Versatility of {l_brace}M(30-crown-10){r_brace} (M = K{sup +}, Ba{sup 2+}) as a guest in UO{sub 2}{sup 2+} complexes of 3.1.3.1 - and 3.3.3 homo-oxa-calixarenes

Energy Technology Data Exchange (ETDEWEB)

Masci, B. [Univ Roma La Sapienza, Dipartimento Chim, I-00185 Rome, (Italy); Thuery, P. [CEA Saclay, DSM/DRECAM/SCM, CNRS-URA 331, F-91191 Gif Sur Yvette, (France)

2007-07-01

The reaction between p-R-[3.1.3.1]- or [3.3.3] homo-oxa-calixarenes and uranyl salts in the presence of 30-crown-10 and the alkali or alkaline-earth metal cations K{sup +} or Ba{sup 2+} gives various supramolecular assemblages characterized by 'complex-within-complex' architectures. These can be of the simple nesting or sandwich types, as in [{l_brace}Ba(30-crown-10){r_brace}{l_brace}UO{sub 2}(L{sup 1}){r_brace}]. 2H{sub 2}O.3CHCl{sub 3} (L{sup 1}H{sub 4} p-tert-butyl[3.1.3.1] homo-oxa-calixarene) and [{l_brace}Ba(30-crown-10){r_brace}{l_brace}UO{sub 2}(L{sup 4}){r_brace}{sub 2}].2CHCl{sub 3} (L{sup 4}H{sub 3} p-bromo[3.3.3]homo-oxa-calixarene), respectively, with the cation held in the cavity of the homo-oxa-calixarene complexes in cone conformation by weak interactions, but more original structures arise when uranyl-cation bonds are present. In [{l_brace}Ba(30-crown-10){r_brace}{l_brace}UO{sub 2}(L{sup 2}){r_brace}] (L{sup 2}H{sub 4} p-phenyl[3.1.3.1] homo-oxa-calixarene), the barium ion included in the crown ether is bound to the uranyl oxo group located out of the calixarene cavity, resulting in the formation of a neutral species which self-organizes to form a columnar assembly by auto-inclusion. In [{l_brace}K(30-crown-10){r_brace}{l_brace}UO{sub 2}K(L{sup 1})(H{sub 2}O){sub 3}{r_brace}]{sub 2}.6H{sub 2}O, the nesting-type subunit dimerizes around two oxo-bound potassium ions. Finally, the use of the coordinating solvent dimethylsulfoxide leads to the neutral complex [UO{sub 2}Ba(L{sup 3})(dmso){sub 2}(MeOH)]{sub 2} (L{sup 3}H{sub 4} = p-methyl[3.1.3.1] homo-oxa-calixarene), in which the crown ether is absent and two oxo-, phenoxo- and ether-bound barium atoms ensure the dimerization of the uranyl complex. (authors)

Synthesis of carbon-11 labeled 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinolinium derivatives as new potential PET SKCa channel imaging agents.

Science.gov (United States)

Gao, Mingzhang; Wang, Min; Zheng, Qi-Huang

2008-02-01

Small conductance Ca2+-activated K+ (SKCa) channels play an important role in many functions such as neuronal communication and behavioral plasticity, secretion, and cell proliferation. SKCa channel modulation is associated with various brain, heart, and cancer diseases. N-methyl-laudanosine and its structurally related derivatives, substituted 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinoliniums, are reversible and selective SKCa channel blockers. Carbon-11 labeled N-methyl-laudanosine and its tetrahydroisoquinolinium derivatives may serve as new probes for positron emission tomography (PET) to image SKCa channels in the brain, heart, and cancer. The key intermediates, substituted isoquinolines (3a-c), were synthesized using a modification of the Pomeranz-Fritsch procedure. The precursors, substituted 1-(3,4-dimethoxybenzyl)-2-methyl-1,2,3,4-tetrahydroisoquinolines (8a-c), and their corresponding reference standards, substituted 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinoliniums (9a-c), were synthesized from compounds 3a-c with 3,4-dimethoxybenzyl chloride (2) in multiple steps with moderate to excellent chemical yields. The precursor 6,7-dimethoxy-1-(3,4-dimethoxybenzyl)-2-methyl-1,2,3,4-tetrahydroisoquinoline (10) was commercially available, and the methylation of compound 10 with methyl iodide provided N-methyl-laudanosine (11). The target quaternary ammonium tracers, carbon-11 labeled 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinoliniums ([11C]9a-c and [11C]11), were prepared by N-[11C]methylation of the tertiary amine precursors (8a-c and 10) with [11C]methyl triflate and isolated by a simplified solid-phase extraction (SPE) purification using a SiO2 or cation-exchange CM Sep-Pak cartridge in 40-65% radiochemical yields.

49 CFR 173.115 - Class 2, Divisions 2.1, 2.2, and 2.3-Definitions.

Science.gov (United States)

2010-10-01

... substances of Class 8, PG I are forbidden from transportation in an aerosol container. (7) Flammable... 2.1, 2.2, and 2.3—Definitions. (a) Division 2.1 (Flammable gas). For the purpose of this subchapter, a flammable gas (Division 2.1) means any material which is a gas at 20 °C (68 °F) or less and 101.3...

2,3-Diphenylmaleimide 1-methylpyrrolidin-2-one monosolvate

Directory of Open Access Journals (Sweden)

Evgeny Bulatov

2014-03-01

Full Text Available In the title compound, C16H11NO2·C5H9NO, the dihedral angles between the maleimide and phenyl rings are 34.7 (2 and 64.8 (2°. In the crystal, the 2,3-diphenylmaleimide and 1-methylpyrrolidin-2-one molecules form centrosymmetrical dimers via pairs of strong N—H...O hydrogen bonds and π–π stacking interactions between the two neighboring maleimide rings [centroid–centroid distance = 3.495 (2 Å]. The dimers are further linked by weak C—H...O and C—H...π hydrogen bonds into a three-dimensional framework.

Protection level of AI H5N1 vaccine clade 2.1.3 commercial against AI H5N1 clade 2.3.2 virus from Ducks to SPF chicken in laboratory conditions

Directory of Open Access Journals (Sweden)

Indriani R

2015-03-01

Full Text Available Highly Pathogenic Avian Influenza (HPAI subtype H5N1 clade 2.3.2 has infected chickens in farms, causing mortality and a decrease in egg production. Vaccination is one of the strategies to control disease of AI subtype H5N1. AI H5N1 clade 2.1.3 vaccine is available commercially. The effectiveness of two vaccines of AI H5N1 clade 2.1.3 (product A and B, and AI H5N1 clade 2.3.2 (Sukoharjo against AI H5N1 clade 2.3.2 (Sukoharjo virus SPF chickens was tested in laboratory. Four groups of SPF chickens were used in this study, there were (1 vaccinated with H5N1 clade 2.1.3 (product A, (2 vaccinated with H5N1 clade 2.1.3 (product B, (3 vaccinated with AI H5N1 clade 2.3.2 and (4 unvaccinated (as a control. Each vaccinated group consisted of 10 chicken except 8 chicken for control group. SPF chicken were vaccinated with 1 dose of vaccine at 3 weeks olds, and then after 3 weeks post vaccination (at 6 weeks olds. All group of chicken were challenged with 106 EID50 per 0.1 ml via intranasal. The results showed, chicken vaccinated with H5N1 clade 2.1.3 product A and B gave 100 and 80% protection respectively, but showed challenged virus shedding, whereas vaccine of H5N1 clade 2.3.2 gave 100% protection from mortality and without virus shedding. Vaccines of AI H5N1 clade 2.1.3 product A was better than vaccine product B, and when chicken vaccinated against H5N1 clade 2.3.2, H5N1 clade 2.3.2 vaccine was the best to be used. In order to protect chicken from AI subtype H5N1 clade 2.1.3 and 2.3.2 in the field, a bivalent vaccine of H5N1 clade 2.1.3 and 2.3.2 subtypes should be developed.

2-(2-Oxo-1,4-dihydro-2H-quinazolin-3-yl)- and 2-(2,2-dioxo-1,4-dihydro-2H-2lambda6-benzo[1,2,6]thiadiazin-3-yl)-N-hydroxy-acetamides as potent and selective peptide deformylase inhibitors.

Science.gov (United States)

Apfel, C; Banner, D W; Bur, D; Dietz, M; Hubschwerlen, C; Locher, H; Marlin, F; Masciadri, R; Pirson, W; Stalder, H

2001-06-07

Potent, selective, and structurally new inhibitors of the Fe(II) enzyme Escherichia coli peptide deformylase (PDF) were obtained by rational optimization of the weakly binding screening hit (5-chloro-2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-acetic acid hydrazide (1). Three-dimensional structural information, gathered from Ni-PDF complexed with 1, suggested the preparation of two series of related hydroxamic acid analogues, 2-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-N-hydroxy-acetamides (A) and 2-(2,2-dioxo-1,4-dihydro-2H-2lambda(6)-benzo[1,2,6]thiadiazin-3-yl)-N-hydroxy-acetamides (B), among which potent PDF inhibitors (37, 42, and 48) were identified. Moreover, two selected compounds, one from each series, 36 and 41, showed good selectivity for PDF over several endoproteases including matrix metalloproteases. However, these compounds showed only weak antibacterial activity.

N-(5-Benzylsulfanyl-1,3,4-thiadiazol-2-yl-2-(piperidin-1-ylacetamide

Directory of Open Access Journals (Sweden)

D. S. Ismailova

2014-03-01

Full Text Available The title compound, C16H20N4OS2, was synthesized by the reaction of 2-benzylsulfanyl-5-chloroacetamido-1,3,4-thiadiazole and piperidine in a 1:2 ratio. The planes of the acetamide and 1,3,4-thiadiazole units are twisted by 10.8 (4°. The thiadiazole S atom and the acetamide O atom are syn-oriented due to a hypervalent S...O interaction of 2.628 (4 Å. In the crystal, molecules form centrosymmetric dimers via N—H...N hydrogen bonds. These dimers are further connected by C—H...O interactions into (100 layers.

Detailed studies of a high-capacity electrode material for rechargeable batteries, Li2MnO3-LiCo(1/3)Ni(1/3)Mn(1/3)O2.

Science.gov (United States)

Yabuuchi, Naoaki; Yoshii, Kazuhiro; Myung, Seung-Taek; Nakai, Izumi; Komaba, Shinichi

2011-03-30

Lithium-excess manganese layered oxides, which are commonly described by the chemical formula zLi(2)MnO(3)-(1-z)LiMeO(2) (Me = Co, Ni, Mn, etc.), are of great importance as positive electrode materials for rechargeable lithium batteries. In this Article, Li(x)Co(0.13)Ni(0.13)Mn(0.54)O(2-δ) samples are prepared from Li(1.2)Ni(0.13)Co(0.13)Mn(0.54)O(2) (or 0.5Li(2)MnO(3)-0.5LiCo(1/3)Ni(1/3)Mn(1/3)O(2)) by an electrochemical oxidation/reduction process in an electrochemical cell to study a reaction mechanism in detail before and after charging across a voltage plateau at 4.5 V vs Li/Li(+). Changes of the bulk and surface structures are examined by synchrotron X-ray diffraction (SXRD), X-ray absorption spectroscopy (XAS), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectroscopy (SIMS). SXRD data show that simultaneous oxygen and lithium removal at the voltage plateau upon initial charge causes the structural rearrangement, including a cation migration process from metal to lithium layers, which is also supported by XAS. This is consistent with the mechanism proposed in the literature related to the Li-excess manganese layered oxides. Oxygen removal associated with the initial charge on the high voltage plateau causes oxygen molecule generation in the electrochemical cells. The oxygen molecules in the cell are electrochemically reduced in the subsequent discharge below 3.0 V, leading to the extra capacity. Surface analysis confirms the formation of the oxygen containing species, such as lithium carbonate, which accumulates on the electrode surface. The oxygen containing species are electrochemically decomposed upon second charge above 4.0 V. The results suggest that, in addition to the conventional transition metal redox reactions, at least some of the reversible capacity for the Li-excess manganese layered oxides originates from the electrochemical redox reaction of the oxygen molecules at the electrode surface.

Efficient Routes to Pyrazolo[3,4-e][1,2,4]triazines and a New Ring System: [1,2,4]Triazino[5,6-d][1,2,3]triazines

Directory of Open Access Journals (Sweden)

Hamad Mohamed Al-Matar

2010-05-01

Full Text Available Arylhydrazonomalononitriles 1a,b react with phenylhydrazine to yield amidrazones 2a,b that cyclize to give 2-aryl-5-phenylhydrazono-2,5-dihydro-[1,2,4]-triazine-6-carbonitriles 5a,b upon reaction with dimethylformamide dimethylacetal (DMFDMA. Refluxing 5a,b in glacial acetic acid resulted in the formation of the pyrazolo-1,2,4-triazines 6a,b. Compounds 6a,b were also formed upon treatment of 3-amino-4-phenylhydrazono-1-phenyl-2-pyrazolin-5-ones 7a,b with DMFDMA. Reacting these triazinyl arylhydrazononitriles 5a,b with hydroxylamine hydrochloride in ethanolic sodium acetate afforded amidrazones 8a,b that are readily cyclized in refluxing dimethylformamide into [1,2,4]triazino[1,2,3]triazines 10a,b.

Excitation mechanisms of 2s1/2-2p3/2 and 2p1/2-2p3/2 transitions in U82+ through U89+

International Nuclear Information System (INIS)

Decaux, V.; Beiersdorfer, P.; Osterheld, A.

1994-01-01

A model based on detailed calculations of the electron-impact excitation of n = 2 electrons in the Li- to Ne-like uranium ions was developed to interpret and explain measurements on EBIT (Electron Beam Ion Trap). While only considering the direct excitation process provided a good model for the electric dipole (El) transitions, it was necessary for the magnetic dipole (Ml) spectrum to include various additional excitation processes in the model. In particular, the model was expanded to include electron-impact excitation of n = 3 levels followed by radiative cascades. Moreover, excitation by the ionization of 2s 1/2 , 2p 1/2 , and 2p 3/2 electrons and by radiative capture of beam electrons into excited levels was added. The new model demonstrates that the dipole-forbidden lines are almost exclusively produced by indirect excitation processes

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.

(2E-3-(4-Chlorophenyl-1-(4-hydroxyphenylprop-2-en-1-one

Directory of Open Access Journals (Sweden)

Jerry P. Jasinski

2011-04-01

Full Text Available In the title compound, C15H11ClO2, the dihedral angle between the mean planes of the chlorobenzene and hydroxybenzene rings is 6.5 (6°. The mean plane of the prop-2-en-1-one group makes an angle of 18.0 (1° with the hydroxyphenyl ring and 11.5 (1° with the chlorophenyl ring. The crystal packing is stabilized by intermolecular O—H...O hydrogen bonds, weak C—H...O, C—H...π and π–π stacking interactions [centroid–centroid distances = 3.7771 (7 and 3.6917 (7 Å].

Annexes 1,2 and 3

International Nuclear Information System (INIS)

2010-01-01

The Annex 1 presents the activities related to ongoing researches within the year of 2010; the Annex 2 presents the internal bylaws of the institution and Annex 3 some additional documents related to all the regulations of the Institute

mer-Bis[3,5-difluoro-2-(2-pyridylphenyl-κ2C1,N]{5-(2-pyridyl-κN-3-[3-(4-vinylbenzyloxyphenyl]-1,2,4-triazol-1-ido}iridium(III methanol solvate

Directory of Open Access Journals (Sweden)

Peter G. Jones

2010-01-01

Full Text Available In the title compound, [Ir(C11H6F2N2(C22H17N4O]·CH3OH, the coordination at iridium is essentially octahedral, but with distortions associated with the bite angles of the ligands [76.25 (9–80.71 (12°] and the differing trans influences of C and N ligands [Ir—N = 2.04 Å (average trans to N but 2.14 Å trans to C]. All three bidentate ligands have coordinating ring systems that are almost coplanar [interplanar angles = 1.7 (1–3.8 (2°]. The vinylbenzyl group is disordered over two positions with occupations of 0.653 (4 and 0.347 (4. The methanol solvent molecule is involved in a classical O—H...N hydrogen bond to a triazole N atom.

CX3CL1/CX3CR1 and CCL2/CCR2 Chemokine/Chemokine Receptor Complex in Patients with AMD

DEFF Research Database (Denmark)

Falk, Mads Krüger; Singh, Amardeep; Faber, Carsten

2014-01-01

PURPOSE: The chemokine receptors CX3CR1 and CCR2 have been implicated in the development of age-related macular degeneration (AMD). The evidence is mainly derived from experimental cell studies and murine models of AMD. The purpose of this study was to investigate the association between expression...... of CX3CR1 and CCR2 on different leukocyte subsets and AMD. Furthermore we measured the plasma levels of ligands CX3CL1 and CCL2. METHODS: Patients attending our department were asked to participate in the study. The diagnosis of AMD was based on clinical examination and multimodal imaging techniques...... positive correlation between CCR2 and CX3CR1 expression on CD8+ cells (r = 0.727, p = 0.0001). We found no difference in plasma levels of CX3CL1 and CCL2 among the groups. CONCLUSIONS: Our results show a down regulation of CX3CR1 on CD8+ cells; this correlated to a low expression of CCR2 on CD8+ cells...

Crystal structure of 1-(2,4-dimethylphenyl-2-(4-trimethylsilyl-1H-1,2,3-triazol-1-ylethanone

Directory of Open Access Journals (Sweden)

G. B. Venkatesh

2014-12-01

Full Text Available The asymmetric unit of the title compound, C15H21N3OSi, contains two molecules with similar conformations (r.m.s. overlay fit for the 20 non-H atoms = 0.163 Å. The dihedral angles between the planes of the 1,2,3-triazole and 2,4-dimethylbenzene rings are 27.0 (3 and 19.5 (3°. In the crystal, molecules are linked by very weak C—H...O and C—H...N hydrogen bonds to generate [100] chains. The chains are cross-linked by C—H...π interactions.

[Hydrogen bis(1,2,4-triazole] 1,2,4-triazolium bis(3-carboxy-4-hydroxybenzenesulfonate 1,2,4-triazole disolvate

Directory of Open Access Journals (Sweden)

Ming-qiang Qiu

2010-08-01

Full Text Available The title compound, C2H4N3+·[H(C2H3N32]+·2C7H5O6S−·2C2H3N3, consists of two types of 1,2,4-triazole monocation, one protonated at the 2-site lying across a twofold axis and the other protonated at the 4-site with the H atom disordered over a center of symmetry, a 5-sulfosalicylate anion and a neutral 1,2,4-triazole molecule. The component ions are linked into a three-dimensional network by a combination of N—H...O, N—H...N, O—H...O, O—H...N, C—H...O and C—H...N hydrogen bonds. In addition, benzene–benzene π–π interactions of 3.942 (2 Å [interplanar spacing = 3.390 (2 Å] and C—O...π (3.331 Å interactions are observed.

A short and facile synthesis of 2-(1Z)-(3-hydroxy-3,7-dimethylocta-1,6-dienyl)-1,4-benzenediol and 1-(3'-methoxypropanoyl)-2,4,5-trimethoxybenzene isolated from Cordia alliodora.

Science.gov (United States)

Kaur, Sukhbir; Singh, Vasundhara; Kumar, Gulshan; Kad, G L; Singh, Jasvinder

2010-03-01

A novel synthesis of 2-(1Z)-(3-hydroxy-3,7-dimethylocta-1,6-dienyl)-1,4-benzenediol and 1-(3'-methoxypropanoyl)-2,4,5-trimethoxybenzene has been carried out by making use of an easily available starting material, acceleration by MW irradiation and the use of water as a green solvent in the key steps.

Synthesis of (R,S)-[2,3-{sup 13}C{sub 2}]-1-(1`-methyl-2`-pyrrolidinyl)propan-2-one; {l_brace}(R,S)-[2`,3`-{sup 13}C{sub 2}]hygrinePound right bracePound

Energy Technology Data Exchange (ETDEWEB)

Abraham, T.W.; Leete, Edward [Minnesota Univ., Minneapolis, MN (United States). Dept. of Chemistry

1996-05-01

2-Ethoxy-1-methyl-5-pyrrolidinone (1) was reacted with ethyl [3,4-{sup 13}C{sub 2}]-acetoacetate (2) in the presence of TiCl{sub 4} to give ethyl [3,4-{sup 13}C{sub 2}]-2-(1`-methyl-5`-oxo-2`-pyrrolidinyl)-3-oxobutanoate (3) in 85% yield. Decarboethoxylation of ethyl [3,4-{sup 13}C{sub 2}]-2-(1`-methyl-5`-oxo-2`-pyrrolidinyl)-3-oxobutan-oate (3) was accomplished using NaCl and H{sub 2}O in DMSO to give (R,S)-[2,3-{sup 13}C{sub 2}]-1-(1`-methyl-5`-oxo-2`-pyrrolidinyl)propan-2-o ne (4) in 91% yield. Protection of the ketone as a ketal (ethylene glycol, H{sup +}), followed by reduction of the amide to the amine using LiAlH{sub 4} and subsequent deprotection of the ketal gave (R,S)-[2,3-{sup 13}C{sub 2}]-1-(1`-methyl-2`-pyrrolidinyl)propan-2-one ((R,s)-[2`, 3`-{sup 13}C{sub 2}]Hygrine) (8) in 78% yield. (61% overall yield from ethyl [3,4-{sup 13}C{sub 2}]acetoacetate). (Author).

Cytotoxicity, genotoxicity, and mutagenicity of 1-chloro-2-hydroxy-3-butene and 1-chloro-3-buten-2-one, two alternative metabolites of 1,3-butadiene

Energy Technology Data Exchange (ETDEWEB)

Liu, Xin-Jie; Zeng, Fang-Mao; An, Jing; Yu, Ying-Xin [Institute of Environmental Pollution and Health, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Zhang, Xin-Yu, E-mail: xyzhang999@shu.edu.cn [Institute of Environmental Pollution and Health, School of Environmental and Chemical Engineering, Shanghai University, Shanghai 200444 (China); Elfarra, Adnan A., E-mail: elfarra@svm.vetmed.wisc.edu [Department of Comparative Biosciences, University of Wisconsin-Madison, Madison, WI 53706 (United States); Molecular and Environmental Toxicology Center, University of Wisconsin-Madison, Madison, WI 53706 (United States)

2013-08-15

The cytotoxicity, genotoxicity, and mutagenicity of 1-chloro-2-hydroxy-3-butene (CHB), a known in vitro metabolite of the human carcinogen 1,3-butadiene, have not previously been investigated. Because CHB can be bioactivated by alcohol dehydrogenases to yield 1-chloro-3-buten-2-one (CBO), a bifunctional alkylating agent that caused globin-chain cross-links in erythrocytes, in the present study we investigated the cytotoxic and genotoxic potential of CHB and CBO in human normal hepatocyte L02 cells using the MTT assay, the relative cloning efficiency assay and the comet assay. We also investigated the mutagenic potential of these compounds with the Ames test using Salmonella strains TA1535 and TA1537. The results provide clear evidence for CHB and CBO being both cytotoxic and genotoxic with CBO being approximately 100-fold more potent than CHB. Interestingly, CHB generated both single-strand breaks and alkali-labile sites on DNA, whereas CBO produced only alkali-labile sites. CHB did not directly result in DNA breaks, whereas CBO was capable of directly generating breaks on DNA. Interestingly, both compounds did not induce DNA cross-links as examined by the comet assay. The Ames test results showed that CHB induced point mutation but not frameshift mutation, whereas the toxic effects of CBO made it difficult to reliably assess the mutagenic potential of CBO in the two strains. Collectively, the results suggest that CHB and CBO may play a role in the mutagenicity and carcinogenicity of 1,3-butadiene. - Highlights: • 1-Chloro-2-hydroxy-3-butene (CHB) is cytotoxic and genotoxic in human liver cells. • The CHB metabolite, 1-chloro-3-buten-2-one (CBO) is ∼ 100-fold more toxic than CHB. • CHB and CBO cause DNA alkali-labile sites, but only CBO directly causes DNA breaks. • CHB is mutagenic in the Ames test, but CBO is too toxic in the assay. • The results suggest a role for CHB in 1,3-butadiene genotoxicity and mutagenicity.

Reactions at the Metal Vertex of a Monometal Metallocarborane Cluster. The Chemistry of (closo-3,3-(PPh3)2-3-(HSO4)-3,1,2-RhC2B9H11) and (closo-3-(PPh3)-3,3-(NO3)-3,1,2RhC2B9H11).

Science.gov (United States)

1982-03-09

4) produced by dissociation of PPh 3 from (2) or through an ionic species such as [closo-3,3- (PPh 3)2 -3,1,2-RhC 289 H ] [HSO4 (4a). Secondly, the...acetylene molecule and subsequent insertion into a metal-carbon bond has been observed in the linear oligomerization of acetylere catalyzed by [Ni(CO...monoxide were obtained from Liquid Carbonic and used without further treatment. Phenylacetylene (Aldrich) was distilled under vacuum before use and n

Effects of Bi(Zn2/3Nb1/3)O3 Modification on the Relaxor Behavior and Piezoelectricity of Pb(Mg1/3Nb2/3)O3-PbTiO3 Ceramics.

Science.gov (United States)

Liu, Zenghui; Wu, Hua; Paterson, Alisa; Ren, Wei; Ye, Zuo-Guang

2017-10-01

Relaxor lead magnesium niobate (PMN)-based materials exhibit complex structures and unusual properties that have been puzzling researchers for decades. In this paper, a new ternary solid solution of Pb(Mg 1/3 Nb 2/3 )O 3 -PbTiO 3 -Bi(Zn 2/3 Nb 1/3 )O 3 (PMN-PT-BZN) is prepared in the form of ceramics, and the effects of the incorporation of BZN into the PMN-PT binary system are investigated. The crystal structure favors a pseudocubic symmetry and the relaxor properties are enhanced as the concentration of BZN increases. The relaxor behavior and the related phase transformations are studied by dielectric spectroscopy. A phase diagram mapping out the characteristic temperatures and various states is established. Interestingly, the piezoelectricity of the PMN-PT ceramics is significantly enhanced by the BZN substitution, with an optimal value of d 33 reaching 826 pC/N for 0.96[0.7Pb(Mg 1/3 Nb 2/3 )O 3 -0.3PbTiO 3 ]-0.04Bi(Zn 2/3 Nb 1/3 )O 3 . This paper provides a better understanding of the relaxor ferroelectric behavior, and unveils a new relaxor-based ternary system as piezoelectric materials potentially useful for electromechanical transducer applications.

Synthesis and Characterization of Mono- and Bicycle Heterocyclic Derivatives Containing 1, 2,4-Triazole, 1,3,4-Thiadiazine and 1,3-Thiazole Rings

Directory of Open Access Journals (Sweden)

Navabeh Nami

2012-01-01

Full Text Available Reaction of tartaric acid with thiocarbohydrazide (2 and thiosemicarbazide (6 afforded 1,2-bis(4-amino-5-mercapto-4H-1,2,4-triazol-3-yl-ethane-1,2-diol (3 and 1,2-bis(5-mercapto-4H-1,2,4-triazol-3-yl-ethane-1,2-diol (7. Reaction of compounds 3 and 7 with DMAD (dimethylacety lendi carboxylate and DEAD (diethylacetylendicarboxylate gave 1,2-bis(7-[(z-methoxycarbonylmethylen]-5,6-dihydro-5H-6-one-[1,2,4] riazolo[3,4-b] [1,3,4] thiadiazin-3-yl-ethan-1,2-diol (4, 1,2-bis(7-[(z-ethoxycarbonylmethylen] -5,6-dihydro -5H-6-one-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazin-3-yl-ethan-1,2- diol (5 and 1,2-bis(6-[(z-methoxycarbonylmethylen]-5-oxo-[1,3]thiazolo[2,3-c] [1,2,4]triazol-3-yl-ethan-1,2-diol (8 in good yields.

Structural and thermal stabilities of layered Li(Ni 1/3Co 1/3Mn 1/3)O 2 materials in 18650 high power batteries

Science.gov (United States)

He, Yan-Bing; Ning, Feng; Yang, Quan-Hong; Song, Quan-Sheng; Li, Baohua; Su, Fangyuan; Du, Hongda; Tang, Zhi-Yuan; Kang, Feiyu

The structural and thermal stabilities of the layered Li(Ni 1/3Co 1/3Mn 1/3)O 2 cathode materials under high rate cycling and abusive conditions are investigated using the commercial 18650 Li(Ni 1/3Co 1/3Mn 1/3)O 2/graphite high power batteries. The Li(Ni 1/3Co 1/3Mn 1/3)O 2 materials maintain their layered structure even when the power batteries are subjected to 200 cycles with 10 C discharge rate at temperatures of 25 and 50 °C, whereas their microstructure undergoes obvious distortion, which leads to the relatively poor cycling performance of power batteries at high charge/discharge rates and working temperature. Under abusive conditions, the increase in the battery temperature during overcharge is attributed to both the reactions of electrolyte solvents with overcharged graphite anode and Li(Ni 1/3Co 1/3Mn 1/3)O 2 cathode and the Joule heat that results from the great increase in the total resistance (R cell) of batteries. The reactions of fully charged Li(Ni 1/3Co 1/3Mn 1/3)O 2 cathodes and graphite anodes with electrolyte cannot be activated during short current test in the fully charged batteries. However, these reactions occur at around 140 °C in the fully charged batteries during oven test, which is much lower than the temperature of about 240 °C required for the reactions outside batteries.

Diaqua[N,N′-bis(2-pyridylmethylenepropane-1,3-diamine]manganese(II dibromide–aquabromido[N,N′-bis(2-pyridylmethylenepropane-1,3-diamine]manganese(II bromide–dibromido[N,N′-bis(2-pyridylmethylenepropane-1,3-diamine]manganese(II (1/2/1

Directory of Open Access Journals (Sweden)

In-Chul Hwang

2009-01-01

Full Text Available There are three different MnII complexes in the asymmetric unit of the title compound, [Mn(C15H16N4(H2O2]Br2·2{[MnBr(C15H16N4(H2O]Br}·[MnBr2(C15H16N4]. In the neutral complex, the Mn2+ ion is six-coordinated in a distorted octahedral environment by four N atoms of the tetradentate ligand N,N′-bis(2-pyridylmethylenepropane-1,3-diamine (bppd and two bromide ligands. In the two cationic complexes, the Mn2+ ions are also six-coordinated in similar environments, but one Mn ion is coordinated by four N atoms of bppd, one Br atom and one O atom of a coordinating water molecule, whereas the other Mn ion is coordinated by four N atoms of bppd and two O atoms of water ligands. The complexes with two coordinated Br atoms or two H2O ligands are disposed about a twofold axis through Mn and C atoms with the special positions ({script{1over 2}}, y, 0 and (0, y, {script{1over 2}}, respectively. The compound displays intermolecular O—H...Br hydrogen bonding. There are intermolecular π–π interactions between adjacent pyridine rings, with centroid–centroid distances of 3.822 and 3.833 Å, and a C—H...O interaction is also present.

Conformance to Generic Letter 83-28, Items 3.1.3 and 3.2.3, Beaver Valley, Unit No. 1, North Anna, Unit Nos. 1 and 2, Surry Unit Nos. 1 and 2 (Docket Nos. 50-334, 50-338, 50-339, 50-280, and 50-281)

International Nuclear Information System (INIS)

Haroldsen, R.

1985-09-01

This report provides a review of the submittals for Beaver Valley, Unit No. 1, North Anna, Unit Nos. 1 and 2, and Surry, Unit Nos. 1 and 2, for conformance to Generic Letter 83-28, Items 3.1.3 and 3.2.3. The specific plants selected were reviewed as a group because of similarity in type and applicability of review items

Study of the structural and thermal stability of Li0.3Co2/3Ni1/6Mn1/6O2

International Nuclear Information System (INIS)

Mahmoud, Abdelfattah; Saadoune, Ismael; Difi, Siham; Sougrati, Moulay Tahar; Lippens, Pierre-Emmanuel; Amarilla, José Manuel

2014-01-01

Thermal and structural stabilities of the delithiated positive electrode material Li x Co 2/3 Ni 1/6 Mn 1/6 O 2 were studied by X-ray diffraction, magnetic and thermogravimetric analysis. In the opposite to the classical electrode materials LiNiO 2 and LiCoO 2 , the structural symmetry (S.G. R-3 m) of the starting material LiCo 2/3 Ni 1/6 Mn 1/6 O 2 is preserved during the electrochemical cycling with a small variation of the unit cell parameters. Squid measurements evidenced that practically no Ni 2+ ions were present in the lithium slab even after the lithium extraction process. For the thermal stability, the highly oxidized phase Li 0.3 Co 2/3 Ni 1/6 Mn 1/6 O 2 was tested. This delithiated phase undergoes only 5.16% weight loss after heating up to 600 °C. This weight loss has no effect on the structure symmetry as the starting α-NaFeO 2 type structure was preserved during the thermal treatment. The obtained results coupled to the excellent electrochemical features of LiCo 2/3 Ni 1/6 Mn 1/6 O 2 clearly showits ability to compete with the commercialized cathode materials

Influence of basis-set size on the X Σ 1 /2 +2 , A Π 1 /2 2 , A Π 3 /2 2 , and B Σ 1 /2 +2 potential-energy curves, A Π 3 /2 2 vibrational energies, and D1 and D2 line shapes of Rb+He

Science.gov (United States)

Blank, L. Aaron; Sharma, Amit R.; Weeks, David E.

2018-03-01

The X Σ 1 /2 +2 , A Π 1 /2 2 , A Π 3 /2 2 , and B2Σ1/2 + potential-energy curves for Rb+He are computed at the spin-orbit multireference configuration interaction level of theory using a hierarchy of Gaussian basis sets at the double-zeta (DZ), triple-zeta (TZ), and quadruple-zeta (QZ) levels of valence quality. Counterpoise and Davidson-Silver corrections are employed to remove basis-set superposition error and ameliorate size-consistency error. An extrapolation is performed to obtain a final set of potential-energy curves in the complete basis-set (CBS) limit. This yields four sets of systematically improved X Σ 1 /2 +2 , A Π 1 /2 2 , A Π 3 /2 2 , and B2Σ1/2 + potential-energy curves that are used to compute the A Π 3 /2 2 bound vibrational energies, the position of the D2 blue satellite peak, and the D1 and D2 pressure broadening and shifting coefficients, at the DZ, TZ, QZ, and CBS levels. Results are compared with previous calculations and experimental observation.

Ho3+/Yb3+ co-doped TeO2-BaF2-Y2O3 glasses for ∼1.2 μm laser applications

Science.gov (United States)

Wang, Shunbin; Li, Chengzhi; Yao, Chuanfei; Jia, Shijie; Jia, Zhixu; Qin, Guanshi; Qin, Weiping

2017-02-01

Intense ∼1.2 μm fluorescence is observed in Ho3+/Yb3+ co-doped TeO2-BaF2-Y2O3 glasses under 915 nm laser diode excitation. The 1.2 μm emission can be ascribed to the transition 5I6→5I8 of Ho3+. With the introducing of BaF2, the content of OH in the glasses drops markedly, and the 1.2 μm emission intensity increases gradually as increasing the concentration percentage of BaF2. Furthermore, microstructured fibers based on the TeO2-BaF2-Y2O3 glasses are fabricated by using a rod-in-tube method, and a relative positive gain of ∼9.42 dB at 1175.3 nm is obtained in a 5 cm long fiber.

Growth and characterization of Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}-Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-PbTiO{sub 3} ternary piezo-/ferroelectric crystals

Energy Technology Data Exchange (ETDEWEB)

Liu, Ying [Key Laboratory of Optoelectronic Materials Chemistry and Physics, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); College of Physics and Energy, Fujian Normal University, Fuzhou, Fujian 350117 (China); He, Chao [Key Laboratory of Optoelectronic Materials Chemistry and Physics, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Yang, Xiaoming [Key Laboratory of Optoelectronic Materials Chemistry and Physics, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); College of Physics and Energy, Fujian Normal University, Fuzhou, Fujian 350117 (China); Li, Xiuzhi; Wang, Zujian [Key Laboratory of Optoelectronic Materials Chemistry and Physics, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Huang, Zhigao; Lai, Fachun [College of Physics and Energy, Fujian Normal University, Fuzhou, Fujian 350117 (China); Long, Xifa, E-mail: lxf@fjirsm.ac.cn [Key Laboratory of Optoelectronic Materials Chemistry and Physics, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

2016-08-05

Piezo-/ferroelectric crystals of Pb(Lu{sub 1/2}Nb{sub 1/2})O{sub 3}-Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-PbTiO{sub 3} ternary solid solution system with high Curie temperature, in the vicinity of morphotropic phase boundary (MPB) region, are grown by the top-seeded solution growth (TSSG) method for the first time. The compositions and structures of the crystals are analyzed, all the structures are found to have pure perovskite structure using X-ray diffraction analysis. Di-/piezo-/ferroelectric properties of the crystals are also characterized systematically. The Curie temperature T{sub c} and coercive field E{sub c}, increase gradually with increasing PbTiO{sub 3} content. In particular, the crystal with composition 0.34PLN-0.31PMN-0.35PT possesses excellent electric properties including the Curie temperature, the rhombohedral–tetragonal phase transition temperature, the piezoelectric coefficient, the remnant polarization and the coercive field, which are T{sub c} = 228 °C, T{sub RT} = 156 °C, d{sub 33} = 2092 pC N{sup −1}, Pr = 35.5 μC cm{sup −2} and E{sub c} = 8.1 kV cm{sup −1}, respectively, making it a promising material for transducers or detectors in a wide temperature range. - Highlights: • PLN-PMN-PT Piezo-/ferroelectric crystals are grown by TSSG method. • The Curie temperature and coercive field increase gradually with increasing PT. • The crystal of 0.34PLN-0.31PMN-0.35PT possesses excellent electric properties.

Photochemistry of 1 and 2-(2-methylphenyl)-1,6-heptadiene. [4a-methyl-1,2,3,4,4a,9,10,10a-octahydrophenanthrene

Energy Technology Data Exchange (ETDEWEB)

Barrows, R.D.; Hornback, J.M.

1982-01-01

In an attempt to synthesize partially saturated phenanthrene derivatives by an intramolecular Diels-Alder reaction between a photochemically produced o-xylylene (diene) and a tethered dienophile, it was found that 1 and 2 underwent a photochemically allowed (2 + 2) cycloaddition. Irradiation of 1 gave 6-(2-methylphenyl)bicyclo(3.2.0)heptane in 86% yield. Upon irradiation of 2, a benzvalene rearrangement of 2 first took place, producing the meta isomer 2-(3-methylphenyl)-1,6-heptadiene, followed by a (2 + 2) photocycloaddition giving 1-(3-methylphenyl)bicyclo(3.2.0)heptane in 15% yield. Direct irradiation of 2-(3-methylphenyl)-1,6-heptadiene gave the same bicyclo derivative as 2 in 34% yield. Examination of the fluorescence spectra of 1 and 2 in comparison with 1-(2-methylphenyl)propene and 2-(2-methylphenyl)-1-butene, respectively, has shown that 1 may be biased toward (2 + 2) cycloaddition where 2 is not biased toward (2 + 2) photocycloization. Attempts to produce 4a-methyl-1,2,3,4,4a,9,10,10a-octahydrophenanthrene by an intramolecular Diels-Alder reaction of the o-xylylene produced by irradiation of 3 will also be described.

A Facile Synthesis of Pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidine and Pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazine Bearing a Thiophene Moiety

Directory of Open Access Journals (Sweden)

Tilal Elsaman

2013-01-01

Full Text Available Pyridinone derivative 8 was synthesized and transformed into the respective chloropyridine 9, which was allowed to react with hydrazine hydrate to afford pyrazolo[3,4-b]pyridin-3-amine derivative 11. Compound 11 was used as a key intermediate for a facile synthesis of the title compounds 14, 15, 17, 21a,b, and 24a–c where the reaction of 11 with some 1,3-dielecrophiles resulted in the formation of pyrido[2′,3′:3,4]pyrazolo[1,5-a]pyrimidines 14, 15, and 17, whereas diazotization of compound 11 gave the respective diazonium salt 18 which was coupled with some active methylene-containing compounds to give the corresponding hydrazones 19a,b and 22a–c. Cyclization of the latter hydrazones yielded the pyrido[2′,3′:3,4]pyrazolo[5,1-c][1,2,4]triazines 21a,b and 24a–c, respectively.

Methyl 3-(Quinolin-2-ylindolizine-1-carboxylate

Directory of Open Access Journals (Sweden)

Roumaissa Belguedj

2015-12-01

Full Text Available A novel compound, methyl 3-(quinolin-2-ylindolizine-1-carboxylate (2 has been synthesized by cycloaddition reaction of 1-(quinolin-2-ylmethylpyridinium ylide (1 with methyl propiolate in presence of sodium hydride in THF. The structure of this compound was established by IR, 1H-NMR, 13C-NMR and MS data

2-Isobutyl-6-(4-methoxyphenylimidazo[2,1-b][1,3,4]thiadiazole

Directory of Open Access Journals (Sweden)

Hoong-Kun Fun

2011-02-01

Full Text Available In the title compound, C15H17N3OS, the dihedral angle between the statistically planar imidazo[2,1-b][1,3,4]thiadiazole fused-ring system (r.m.s. deviation = 0.002 Å and the methyoxbenzene ring is 4.52 (6°. In the crystal, molecules are arranged into columns and stacked down the a axis. The crystal structure is stabilized by weak C—H...π and π–π interactions [centroid–centroid separations = 3.6053 (8 and 3.7088 (7 Å].

5,5-Dimethyl-2-methylseleno-1,3,2-dioxaphosphorinan-2-one

Directory of Open Access Journals (Sweden)

Grzegorz Cholewinski

2010-04-01

Full Text Available The title compound, C6H13O3PSe, was obtained in the reaction of 5,5-dimethyl-2-oxo-2-seleno-1,3,2-dioxaphosphorinane potassium salt with methyl iodide. The selenomethyl group is in the axial position in relation to the six-membered dioxaphosphorinane ring.

Hydrothermal synthesis of layered Li[Ni1/3Co1/3Mn1/3]O2 as positive electrode material for lithium secondary battery

International Nuclear Information System (INIS)

Myung, Seung-Taek; Lee, Myung-Hun; Komaba, Shinichi; Kumagai, Naoaki; Sun, Yang-Kook

2005-01-01

In attempts to prepare layered Li[Ni 1/3 Co 1/3 Mn 1/3 ]O 2 , hydrothermal method was employed. The hydrothermal precursor, [Ni 1/3 Co 1/3 Mn 1/3 ](OH) 2 , was synthesized via a coprecipitation route. The sphere-shaped powder precursor was hydrothermally reacted with LiOH aqueous solution at 170 deg. C for 4 days in autoclave. From X-ray diffraction and scanning electron microscopic studies, it was found that the as-hydrothermally prepared powders were crystallized to layered α-NaFeO 2 structure and the particles had spherical shape. The as-prepared Li[Ni 1/3 Co 1/3 Mn 1/3 ]O 2 delivered an initial discharge of about 110 mA h g -1 due to lower crystallinity. Heat treatment of the hydrothermal product at 800 deg. C was significantly effective to improve the structural integrity, which consequently affected the increase in the discharge capacity to 157 (4.3 V cut-off) and 182 mA h g -1 (4.6 V cut-off) at 25 deg. C with good reversibility

CuO-Nanoparticles Catalyzed Synthesis of 1,4-Disubstituted-1,2,3 ...

Indian Academy of Sciences (India)

John Paul Raj

2018-04-13

Apr 13, 2018 ... has been developed for the synthesis of 1,2,3-triazoles. A library of 1 ... Kuang et al., described Cu-catalyzed synthesis of 1H-. 1,2,3-triazoles from 1 ..... Tornøe C W, Christensen C and Meldal M 2002 Peptido- triazoles on solid ... 2015 Copper-catalyzed [3+2] cycloaddition/oxidation reactions between ...

Urchin-Like Ni1/3Co2/3(CO3)1/2(OH)·0.11H2O for Ultrahigh-Rate Electrochemical Supercapacitors: Structural Evolution from Solid to Hollow.

Science.gov (United States)

Wei, Wutao; Cui, Shizhong; Ding, Luoyi; Mi, Liwei; Chen, Weihua; Hu, Xianluo

2017-11-22

Portable electronics and electric or hybrid electric vehicles are developing in the trend of fast charge and long electric mileage, which ask us to design a novel electrode with sufficient electronic and ionic transport channels at the same time. Herein, we fabricate a uniform hollow-urchin-like Ni 1/3 Co 2/3 (CO 3 ) 1/2 (OH)·0.11H 2 O electrode material through an easy self-generated and resacrificial template method. The one-dimensional chain-like crystal structure unit containing the metallic bonding and the intercalated OH - and H 2 O endow this electrode material with abundant electronic and ionic transport channels. The hollow-urchin-like structure built by nanorods contributes to the large electrode-electrolyte contact area ensuring the supply of ions at high current. CNTs are employed to transport electrons between electrode material and current collector. The as-assembled NC-CNT-2//AC supercapacitor device exhibits a high specific capacitance of 108.3 F g -1 at 20 A g -1 , a capacitance retention ratio of 96.2% from 0.2 to 20 A g -1 , and long cycle life. Comprehensive investigations unambiguously highlight that the unique hollow-urchin-like Ni 1/3 Co 2/3 (CO 3 ) 1/2 (OH)·0.11H 2 O electrode material would be the right candidate for advanced next-generation supercapacitors.

Conformational analysis and global warming potentials of 1,1,1,3,3,3-hexafluoro-2-propanol from absorption spectroscopy

Science.gov (United States)

Godin, Paul J.; Le Bris, Karine; Strong, Kimberly

2017-12-01

Absorption cross-sections of 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) were derived from Fourier transform infrared spectra recorded from 530 to 3400 cm-1 with a resolution of 0.1 cm-1 over a temperature range of 300-362 K. These results were compared to previously published experimental measurements made at room temperature and to a theoretical spectrum from density functional theory (DFT) calculations. Good agreement is found between the experimentally derived results, DFT calculations, and previously published data. The only temperature dependence observed was in the amplitude of some of the absorption peaks due to the changing ratio of the stable conformations of HFIP. This temperature dependence does not result in a significant trend in integrated band strength as a function of temperature. The average value for integrated band strength is found to be (2.649 ± 0.065)x10-16 cm molecule-1 for HFIP over the spectral range of 595 to 3010 cm-1. Radiative efficiency (RE) and the global warming potential (GWP) for HFIP were also derived. A RE of 0.293 ± 0.059 Wm-2ppbv-1 is derived, which leads to a GWP100 of 188 in the range of 530 to 3000 cm-1. The DFT calculation is linearly adjusted to match the experimental spectrum. Using this adjusted DFT spectrum to expand the range below 530 to 0 cm-1 , increases the RE to 0.317 ± 0.063 Wm-2ppbv-1 and the GWP100 to 203.

3-{2-[(3-{(E-2-[4-(Dimethylaminophenyl]ethenyl}quinoxalin-2-yloxy]ethyl}-1,3-oxazolidin-2-one monohydrate

Directory of Open Access Journals (Sweden)

Youssef Ramli

2012-01-01

Full Text Available In the title compound, C23H24N4O3·H2O, the 1,3-oxazoline ring is nearly planar [maximum deviation = 0.059 (2 Å] and its mean plane is twisted by 30.12 (8° with respect to the quinoxaline fused-ring system; the benzene ring is nearly coplanar with the quinoxaline fused-ring system [dihedral angle = 2.52 (2°]. The water molecule of crystallization is hydrogen-bond donor to an N atom of the quinoxaline ring system as well as an O atom of the oxazolinone unit, the two hydrogen bonds generating a chain running along the c axis.

3-Methyl-1-(prop-2-en-1-ylquinoxalin-2(1H-one

Directory of Open Access Journals (Sweden)

Youssef Ramli

2010-07-01

Full Text Available In the molecule of the title compound, C12H12N2O, the quinoxaline ring is planar with an r.m.s. deviation of 0.007 (15 Å. The dihedral angle between the quinoxaline and propenyl planes is 82.1 (2°. The crystal packing is stabilized by offset π–π stacking between the quinoxaline rings [centroid–centroid distance = 3.8832 (9 Å].

Synthesis of Some New 1,3,4-Thiadiazole, Thiazole and Pyridine Derivatives Containing 1,2,3-Triazole Moiety

Directory of Open Access Journals (Sweden)

Nadia A. Abdelriheem

2017-02-01

Full Text Available In this study, 1-(5-Methyl-1-(p-tolyl-1H-1,2,3-triazol-4-ylethan-1-one, was reacted with Thiosemicarbazide, alkyl carbodithioate and benzaldehyde to give thiosemicarbazone, alkylidenehydrazinecarbodithioate and 3-phenylprop-2-en-1-one-1,2,3-triazole derivatives. The 1,3,4-thiadiazole derivatives containing the 1,2,3-triazole moiety were obtained via reaction of alkylidenecarbodithioate with hydrazonoyl halides. Also, hydrazonoyl halides were reacted with thiosemicarbazone and pyrazolylthioamide to give 1,3-thiazoles derivatives. Subsequently, 3-phenyl2-en-1-one was used to synthesize substituted pyridines and substituted nicotinic acid ester. The latter was converted to its azide compound which was reacted with aromatic amines and phenol to give substituted urea and phenylcarbamate containing 1,2,3-triazole moiety. The newly synthesized compounds were established by elemental analysis, spectral data and alternative synthesis whenever possible.

Synthesis and antitumoral activity of novel 3-(2-substituted-1,3,4-oxadiazol-5-yl) and 3-(5-substituted-1,2,4-triazol-3-yl) beta-carboline derivatives.

Science.gov (United States)

Formagio, Anelise S Nazari; Tonin, Lilian T Düsman; Foglio, Mary Ann; Madjarof, Christiana; de Carvalho, João Ernesto; da Costa, Willian Ferreira; Cardoso, Flávia P; Sarragiotto, Maria Helena

2008-11-15

Several novel 1-substituted-phenyl beta-carbolines bearing the 2-substituted-1,3,4-oxadiazol-5-yl and 5-substituted-1,2,4-triazol-3-yl groups at C-3 were synthesized and evaluated for their in vitro anticancer activity. The assay results pointed thirteen compounds with growth inhibition effect (GI(50)<100 microM) for all eight different types of human cancer cell lines tested. The beta-carbolines 7a and 7h, bearing the 3-(2-metylthio-1,3,4-oxadiazol-5-yl) group, displayed high selectivity and potent anticancer activity against ovarian cell line with GI(50) values lying in the nanomolar concentration range (GI(50)=10 nM for both compounds). The 1-(N,N-dimethylaminophenyl)-3-(5-thioxo-1,2,4-triazol-3-yl) beta-carboline (8g) was the most active compound, showing particular effectiveness on lung (GI(50)=0.06 microM), ovarian and renal cell lines. The potent anticancer activity presented for synthesized compounds 7a, 7h, and 8g, together with their easiness of synthesis, makes these compounds promising anticancer agents.

1,1′-{1,4-Phenylene bis[3-(6-chloro-2-methyl-4-phenylquinolin-3-yl-4,5-dihydro-1H-pyrazole-5,1-diyl]}dibutan-1-one

Directory of Open Access Journals (Sweden)

Allaoua Kedjadja

2015-10-01

Full Text Available A new polycyclic compound, 1,1′-{1,4-phenylene bis[3-(6-chloro-2-methyl-4-phenylquinolin-3-yl-4,5-dihydro-1H-pyrazole-5,1-diyl]}dibutan-1-one (3 has been synthesized by cyclocondensation of (2E,2′E-1,1′-bis(6-chloro-2-methyl-4-phenylquinolin-3-yl-3,3′-(1,4-phenylenediprop-2-en-1-one (2 and hydrazine hydrate in butanoic acid. The structure of this compound was established by elemental analysis, 1H-NMR, 13C-NMR, mass and IR spectroscopy.

Pot-Economy Autooxidative Condensation of 2-Aryl-2-lithio-1,3-dithianes.

Science.gov (United States)

Vale, João R; Rimpiläinen, Tatu; Sievänen, Elina; Rissanen, Kari; Afonso, Carlos A M; Candeias, Nuno R

2018-02-16

The autoxidative condensation of 2-aryl-2-lithio-1,3-dithianes is here reported. Treatment of 2-aryl-1,3-dithianes with n-BuLi in the absence of any electrophile leads to condensation of three molecules of 1,3-dithianes and formation of highly functionalized α-thioether ketones orthothioesters in 51-89% yields upon air exposure. The method was further expanded to benzaldehyde dithioacetals, affording corresponding orthothioesters and α-thioether ketones in 48-97% yields. The experimental results combined with density functional theory studies support a mechanism triggered by the autoxidation of 2-aryl-2-lithio-1,3-dithianes to yield a highly reactive thioester that undergoes condensation with two other molecules of 2-aryl-2-lithio-1,3-dithiane.

Synthesis, structure, luminescent, and magnetic properties of carbonato-bridged Zn(II)2Ln(III)2 complexes [(μ4-CO3)2{Zn(II)L(n)Ln(III)(NO3)}2] (Ln(III) = Gd(III), Tb(III), Dy(III); L(1) = N,N'-bis(3-methoxy-2-oxybenzylidene)-1,3-propanediaminato, L(2) = N,N'-bis(3-ethoxy-2-oxybenzylidene)-1,3-propanediaminato).

Science.gov (United States)

Ehama, Kiyomi; Ohmichi, Yusuke; Sakamoto, Soichiro; Fujinami, Takeshi; Matsumoto, Naohide; Mochida, Naotaka; Ishida, Takayuki; Sunatsuki, Yukinari; Tsuchimoto, Masanobu; Re, Nazzareno

2013-11-04

Carbonato-bridged Zn(II)2Ln(III)2 complexes [(μ4-CO3)2{Zn(II)L(n)Ln(III)(NO3)}2]·solvent were synthesized through atmospheric CO2 fixation reaction of [Zn(II)L(n)(H2O)2]·xH2O, Ln(III)(NO3)3·6H2O, and triethylamine, where Ln(III) = Gd(III), Tb(III), Dy(III); L(1) = N,N'-bis(3-methoxy-2-oxybenzylidene)-1,3-propanediaminato, L(2) = N,N'-bis(3-ethoxy-2-oxybenzylidene)-1,3-propanediaminato. Each Zn(II)2Ln(III)2 structure possessing an inversion center can be described as two di-μ-phenoxo-bridged {Zn(II)L(n)Ln(III)(NO3)} binuclear units bridged by two carbonato CO3(2-) ions. The Zn(II) ion has square pyramidal coordination geometry with N2O2 donor atoms of L(n) and one oxygen atom of a bridging carbonato ion at the axial site. Ln(III) ion is coordinated by nine oxygen atoms consisting of four from the deprotonated Schiff-base L(n), two from a chelating nitrate, and three from two carbonate groups. The temperature-dependent magnetic susceptibilities in the range 1.9-300 K, field-dependent magnetization from 0 to 5 T at 1.9 K, and alternating current magnetic susceptibilities under the direct current bias fields of 0 and 1000 Oe were measured. The magnetic properties of the Zn(II)2Ln(III)2 complexes are analyzed on the basis of the dicarbonato-bridged binuclear Ln(III)-Ln(III) structure, as the Zn(II) ion with d(10) electronic configuration is diamagnetic. ZnGd1 (L(1)) and ZnGd2 (L(2)) show a ferromagnetic Gd(III)-Gd(III) interaction with J(Gd-Gd) = +0.042 and +0.028 cm(-1), respectively, on the basis of the Hamiltonian H = -2J(Gd-Gd)ŜGd1·ŜGd2. The magnetic data of the Zn(II)2Ln(III)2 complexes (Ln(III) = Tb(III), Dy(III)) were analyzed by a spin Hamiltonian including the crystal field effect on the Ln(III) ions and the Ln(III)-Ln(III) magnetic interaction. The Stark splitting of the ground state was so evaluated, and the energy pattern indicates a strong easy axis (Ising type) anisotropy. Luminescence spectra of Zn(II)2Tb(III)2 complexes were observed, while those

N,N,N′,N′,N′′,N′′-Hexamethylguanidinium 1,1,3,3-tetracyanoprop-2-en-1-ide

Directory of Open Access Journals (Sweden)

Ioannis Tiritiris

2016-03-01

Full Text Available The asymmetric unit of the title salt, C7H18N3+·C7HN4−, comprises one cation and one anion. The N,N,N′,N′,N′′,N′′-hexamethylguanidinium ion shows orientational disorder and two sets of N- and C-atom positions were found, with an occupancy ratio of 0.535 (3:0.465 (3. The C—N bond lengths in the guanidinium ion range from 1.339 (16 to 1.35 (2 Å, indicating partial double-bond character pointing towards charge delocalization within the NCN planes. The negative charge in the 1,1,3,3-tetracyanoprop-2-en-1-ide ion is delocalized within the CCC planes with the C—C bonds ranging in length from 1.379 (3 to 1.427 (3 Å, also indicating partial double-bond character.

Synthesis and Biological Activity of 3-(2-Furanyl-6-Aryl-1,2,4-Triazolo[3,4-b]-1,3,4 –Thiadiazoles

Directory of Open Access Journals (Sweden)

Zi-Yi Zhang

2002-08-01

Full Text Available 3-(2-Furanyl-4-amino-5-mercapto-1,2,4-triazole (1 was prepared from 2-furoic acid through a multi-step reaction sequence. Compound 1 reacted with aromatic acids in the presence of phosphorus oxychloride to give 3-(2-furanyl-6-aryl-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles (2. The structures of all the newly synthesized compounds have been confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR and mass spectra. The bioassay indicated most of the title compounds possess significant growth promoting effects on mung bean radicles.

Atmospheric chemistry of n-CxF2x+1CHO (x = 1, 2, 3, 4)

DEFF Research Database (Denmark)

Hurley, M. D.; Ball, J. C.; Wallington, T. J.

2006-01-01

Smog chamber/FTIR techniques were used to study the atmospheric fate of n-C(x)F(2)(x)(+1)C(O) (x = 1, 2, 3, 4) radicals in 700 Torr O(2)/N(2) diluent at 298 +/- 3 K. A competition is observed between reaction with O(2) to form n-C(x)()F(2)(x)()(+1)C(O)O(2) radicals and decomposition to form n-C(x...... to the atmospheric chemistry of n-C(x)F(2)(x)(+1)C(O) radicals and their possible role in contributing to the formation of perfluorocarboxylic acids in the environment....

Propane-1,3-diaminium–2-carboxypyridine-6-carboxylate–pyridine-2,6-dicarboxylic acid–water (1/2/2/8

Directory of Open Access Journals (Sweden)

Hossein Aghabozorg

2008-01-01

Full Text Available The title proton-transfer compound, C3H12N22+·2C7H4NO4−·2C7H5NO4·8H2O or (pnH2(pydcH2.2(pydcH2·8H2O, was obtained by the reaction of pyridine-2,6-dicarboxylic acid (pydcH2 and propane-1,3-diamine (pn in aqueous solution. Both neutral and monoanionic forms of the diacid are observed in the crystal structure. The negative charge of two monoanions is balanced by the dicationic propane-1,3-diaminium species. In addition, considerable π–π stacking interactions between the aromatic rings of the (pydcH− and (pydcH2 fragments [with centroid–centroid distances of 3.5108 (11–3.5949 (11 Å] are observed. The most important feature of this crystal structure is the presence of a large number of O—H...O, O—H...N, N—H...O, N—H...N, C—H...O and C—H...N hydrogen bonds, with D...A ranging from 2.445 (2 to 3.485 (3 Å. These interactions as well as ion pairing and π–π stacking connect the various fragments into a supramolecular structure.

Leaching process for recovering valuable metals from the LiNi1/3Co1/3Mn1/3O2 cathode of lithium-ion batteries.

Science.gov (United States)

He, Li-Po; Sun, Shu-Ying; Song, Xing-Fu; Yu, Jian-Guo

2017-06-01

In view of the importance of environmental protection and resource recovery, recycling of spent lithium-ion batteries (LIBs) and electrode scraps generated during manufacturing processes is quite necessary. An environmentally sound leaching process for the recovery of Li, Ni, Co, and Mn from spent LiNi 1/3 Co 1/3 Mn 1/3 O 2 -based LIBs and cathode scraps was investigated in this study. Eh-pH diagrams were used to determine suitable leaching conditions. Operating variables affecting the leaching efficiencies for Li, Ni, Co, and Mn from LiNi 1/3 Co 1/3 Mn 1/3 O 2 , such as the H 2 SO 4 concentration, temperature, H 2 O 2 concentration, stirring speed, and pulp density, were investigated to determine the most efficient conditions for leaching. The leaching efficiencies for Li, Ni, Co, and Mn reached 99.7% under the optimized conditions of 1M H 2 SO 4 , 1vol% H 2 O 2 , 400rpm stirring speed, 40g/L pulp density, and 60min leaching time at 40°C. The leaching kinetics of LiNi 1/3 Co 1/3 Mn 1/3 O 2 were found to be significantly faster than those of LiCoO 2 . Based on the variation in the weight fraction of the metal in the residue, the "cubic rate law" was revised as follows: θ(1-f) 1/3 =(1-kt/r 0 ρ), which could characterize the leaching kinetics optimally. The activation energies were determined to be 64.98, 65.16, 66.12, and 66.04kJ/mol for Li, Ni, Co, and Mn, respectively, indicating that the leaching process was controlled by the rate of surface chemical reactions. Finally, a simple process was proposed for the recovery of valuable metals from spent LiNi 1/3 Co 1/3 Mn 1/3 O 2 -based LIBs and cathode scraps. Copyright © 2017 Elsevier Ltd. All rights reserved.

{[2-Methyl-2-(phenoxymethylpropane-1,3-diyl]bis(oxy}dibenzene

Directory of Open Access Journals (Sweden)

Ziad Moussa

2014-05-01

Full Text Available The title compound, C23H24O3, was obtained in a one-step (60% yield synthesis from 1,1,1-tris(hydroxymethylethane. It features a tripodal ligand capable of complexing metal centres. One of the three conformations involving the methyl group, the central C—C bond and the phenoxy substituents is antiperiplanar while the two others are synclinal [the corresponding C—C—C—O torsion angles are −174.6 (1, −53.2 (2 and −47.3 (2°]. In the crystal, C—H...O interactions link the molecules into [010] chains.

Thermodynamic properties of 1-ethyl-4-nitro-1,2,3-triazole

Energy Technology Data Exchange (ETDEWEB)

Blokhin, Andrey V., E-mail: blokhin@bsu.by; Kohut, Sviataslau V.; Kabo, Gennady J.; Stepurko, Elena N.; Paulechka, Yauheni U.; Voitkevich, Olga V.

2013-08-10

Graphical abstract: - Highlights: • Heat capacities and phase transition enthalpies for 1-ethyl-4-nitro-1,2,3-triazole were measured. • Enthalpy of formation for 1-ethyl-4-nitro-1,2,3-triazole was determined. • Vapor pressure and enthalpy of sublimation of 1-ethyl-4-nitro-1,2,3-triazole were found from Knudsen measurements. - Abstract: Temperature dependence of the heat capacity and the parameters of phase transitions of 1-ethyl-4-nitro-1,2,3-triazole (1ET) were studied between 5 and 370 K in a vacuum adiabatic calorimeter. Thermodynamic properties of the 1ET in the condensed state were obtained over the range of 0–370 K. Saturated vapor pressure for crystalline 1ET in the temperature ranges from 313 to 344 K and its enthalpy of sublimation were measured by the Knudsen effusion method. The standard enthalpy of formation for crystalline 1ET at 298.15 K was determined in a static bomb combustion calorimeter. From these data, the standard enthalpy of formation for gaseous 1ET was evaluated. The enthalpy of formation calculated using quantum chemical methods is in excellent agreement with the experimental value.

Thermodynamic properties of 1-ethyl-4-nitro-1,2,3-triazole

International Nuclear Information System (INIS)

Blokhin, Andrey V.; Kohut, Sviataslau V.; Kabo, Gennady J.; Stepurko, Elena N.; Paulechka, Yauheni U.; Voitkevich, Olga V.

2013-01-01

Graphical abstract: - Highlights: • Heat capacities and phase transition enthalpies for 1-ethyl-4-nitro-1,2,3-triazole were measured. • Enthalpy of formation for 1-ethyl-4-nitro-1,2,3-triazole was determined. • Vapor pressure and enthalpy of sublimation of 1-ethyl-4-nitro-1,2,3-triazole were found from Knudsen measurements. - Abstract: Temperature dependence of the heat capacity and the parameters of phase transitions of 1-ethyl-4-nitro-1,2,3-triazole (1ET) were studied between 5 and 370 K in a vacuum adiabatic calorimeter. Thermodynamic properties of the 1ET in the condensed state were obtained over the range of 0–370 K. Saturated vapor pressure for crystalline 1ET in the temperature ranges from 313 to 344 K and its enthalpy of sublimation were measured by the Knudsen effusion method. The standard enthalpy of formation for crystalline 1ET at 298.15 K was determined in a static bomb combustion calorimeter. From these data, the standard enthalpy of formation for gaseous 1ET was evaluated. The enthalpy of formation calculated using quantum chemical methods is in excellent agreement with the experimental value

Poly[(μ4-biphenyl-3,3′-dicarboxylatobis[μ2-1,1′-(butane-1,4-diyldiimidazole](μ2-oxalatodimanganese(II

Directory of Open Access Journals (Sweden)

Bao-Yong Zhu

2010-10-01

Full Text Available In the title coordination compound, [Mn2(C14H8O4(C2O4(C10H14N42]n, the biphenyl-3,3′-dicarboxylate and oxalate anions, both situated on inversion centres, function in a bridging mode, linking the dinuclear MnII atoms into wave-like layers. Each 1,1′-(1,4-butane-1,4-diyldiimidazole ligand coordinates to two MnII atoms located in adjacent layers via Mn—N coordination bonds, giving a three-dimensional network. As the methylene groups can bend freely relative to each other due to the C atoms connected via single bonds, the 1,1′-(butane-1,4-diyldiimidazole ligand forms an S-shaped conformation, which makes the void in the three-dimensional network distorted.

(E-Methyl 3-(3,4-dimethoxyphenyl-2-[(1,3-dioxoisoindolin-2-ylmethyl]acrylate

Directory of Open Access Journals (Sweden)

D. Kannan

2012-04-01

Full Text Available In the title compound, C21H19NO6, the isoindole ring system is essentially planar [maximum deviation = 0.019 (2 Å for the N atom] and is oriented at a dihedral angle of 51.3 (1° with respect to the benzene ring. The two methoxy groups are almost coplanar with the attached benzene ring [C—O—C—C = 3.7 (4 and 4.3 (4°]. The molecular conformation is stabilized by an intramolecular C—H...O hydrogen bond, which generates an S(9 ring motif. In the crystal, molecules are linked through bifurcated C—H...(O,O hydrogen bonds having R12(5 ring motifs, forming chains along the b-axis direction. The crystal packing is further stabilzed by π–π interactions [centriod–centroid distance = 3.463 (1 Å].

Efficient Synthesis of 1-Sulfonyl-1,2,3-triazoles

Science.gov (United States)

Raushel, Jessica; Fokin, Valery V.

2010-01-01

An efficient room temperature method for the synthesis of 1-sulfonyl-1,2,3-triazoles from in situ generated copper(I) acetylides and sulfonyl azides is described. Copper(I) thiophene-2-carboxylate (CuTC) catalyst produces the title compounds under both non-basic anhydrous and aqueous conditions in good yields. PMID:20931987

New Pb(Mg1/3Nb2/3)O3-Pb(In1/2Nb1/2)O3-PbZrO3-PbTiO3 Quaternary Ceramics: Morphotropic Phase Boundary Design and Electrical Properties.

Science.gov (United States)

Luo, Nengneng; Zhang, Shujun; Li, Qiang; Xu, Chao; Yang, Zhanlue; Yan, Qingfeng; Zhang, Yiling; Shrout, Thomas R

2016-06-22

Four series of Pb(Mg1/3Nb2/3)O3-Pb(In1/2Nb1/2)O3-PbZrO3-PbTiO3 (PMN-PIN-PZ-PT) quaternary ceramics with compositions located at the morphotropic phase boundary (MPB) regions were prepared. The MPBs of the multicomponent system were predicted using a linear combination rule and experimentally confirmed by X-ray powder diffraction and electrical measurement. The positions of MPBs in multicomponent systems were found in linear correlation with the tolerance factor and ionic radii of non-PT end-members. The phase structure, piezoelectric coefficient, electromechanical coupling coefficient, unipolar strains, and dielectric properties of as-prepared ceramics were systematically investigated. The largest d33s were obtained at S36.8, L37.4, M39.6, and N35.8, with the corresponding values of 580, 450, 420, and 530 pC/N, respectively, while the largest kps were found at S34.8, L37.4, M39.6, and N35.8, with the respective values of 0.54, 0.50, 0.47, and 0.53. The largest unipolar strain Smax and high-field piezoelectric strain coefficients d33* were also observed around the respective MPB regions. The rhombohedral-to-tetragonal phase transition temperature Trt increased with increasing PIN and PZ contents. Of particular importance is that high Trt of 140-197 °C was achieved in the M series with PZ and PIN contents being around 0.208 and 0.158, which will broaden the temperature usage range.

Synthesis of 14C- and 2H-labeled 1,3 dihydro-3, 3-dimethyl-5-(1,4,5,6,- tetrahydro-6-oxo-3-pyridazinyl)-2H-indol-2-one (LY195115), an orally effective positive inotrope

International Nuclear Information System (INIS)

Robertson, D.W.; Krushinski, J.H.; Kau, D.

1986-01-01

The synthesis of 14 C- and 2 H-labeled 1,3-dihydro-3,3-dimethyl-5-(1,4,5,6-tetrahydro-6-oxo-3-pyridazinyl)-2H-indol -2-one (LY195115), an extremely potent, orally-effective cardiotonic with inotropic and vasodilator activities is described. The 14 C-label was introduced in the antepenultimate step by reaction of a β-chloroketone precursor with Na 14 CN; acid-catalyzed hydrolysis and cyclization with hydrazine provided the tetrahydropyridazinone bearing the 14 C-label in the oxo-carbon. 1,3-Dihydro-3,3-di(methyl-d 3 ) -2H-indol-2-one was prepared by exhaustive methylation of 1-acetyl-1,3-dihydro-2H-indol-2-one with sodium hydride and iodomethane-d 3 , followed by removal of the nitrogen protecting group. This labeled material was converted in two steps to [ 2 H 6 ]-LY195115. (author)

Electrical and magnetic properties of 0-3 Ba(Fe1/2Nb1/2)O3/PVDF composites

Science.gov (United States)

Ranjan, Hars; Mahto, Uttam K.; Chandra, K. P.; Kulkarni, A. R.; Prasad, A.; Prasad, K.

Lead-free Ba(Fe1/2Nb1/2)O3/PVDF 0-3 composites were fabricated using melt-mixing technique. X-ray diffraction, scanning electron microscopy, dielectric, impedance, ac conductivity, magnetic force microscopy (MFM) and vibrating sample magnetometer studies were undertaken to characterize the samples. Average crystallite size of the Ba(Fe1/2Nb1/2)O3 powder, estimated using Williamson-Hall approach, was found to be ˜42nm. The filler particles of ˜0.5-1μm were found to disperse in the polymer matrix of all the composites. Filler concentration-dependent values of real and imaginary parts of complex permittivity showed increasing trend and were seen to follow Bruggeman and Furukawa equations. The data for ac conductivity exhibited negative temperature coefficient of resistance character of the test materials and were found to obey Jonscher’s power law. The correlated barrier hopping model was found to explain satisfactorily the mechanism of charge transport occurring in the system. MFM confirmed the presence of magnetic phases in the composites. Typical magnetization versus applied field curves indicated the possibility of magnetoelectric coupling in the system. Hence, the present composites have shown themselves as potential multi-functional candidate materials for use in high density data storage applications.

Volatility study of [C1C1im][NTf2] and [C2C3im][NTf2] ionic liquids

International Nuclear Information System (INIS)

Rocha, Marisa A.A.; Ribeiro, Filipe M.S.; Schröder, Bernd; Coutinho, João A.P.; Santos, Luís M.N.B.F.

2014-01-01

Highlights: • Vapor pressures of [C 1 C 1 im][NTf 2 ] and [C 2 C 3 im][NTf 2 ] ionic liquids are reported. • [C 1 C 1 im][NTf 2 ] presents higher enthalpy and entropy of vaporization than expected. • The high volatility of [C 2 C 3 im][NTf 2 ] is a result from its asymmetric character. -- Abstract: Vapor pressures of 1,3-dimethylimidazolium bis(trifluoromethylsulfonyl)imide, ([C 1 C 1 im][NTf 2 ]) and 1-ethyl-3-propylimidazolium bis(trifluoromethylsulfonyl)imide, ([C 2 C 3 im][NTf 2 ]) ionic liquids were measured as a function of temperature using a Knudsen effusion apparatus combined with a quartz crystal microbalance. Enthalpies and entropies of vaporization were derived from the fitting of vapor pressure and temperature results to the Clarke and Glew equation. [C 1 C 1 im][NTf 2 ] presents a higher enthalpy and entropy of vaporization than the neighboring members of the series. The enthalpy of vaporization of [C 2 C 3 im][NTf 2 ] lies in between the asymmetric and symmetric ionic liquid series, reflecting a decrease in the electrostatic interactions due to a decrease of the charge accessibility between the ionic pairs when the methyl group is replaced by an ethyl group. The obtained higher volatility of [C 2 C 3 im][NTf 2 ] arises from its asymmetric character, leading to an higher entropic contribution that compensates the enthalpic penalty. The border conditions ([C 1 C 1 im][NTf 2 ], [C 2 C 1 im][NTf 2 ] and [C 2 C 2 im][NTf 2 ]), topology ([C 2 C 3 im][NTf 2 ]) and symmetry/asymmetry of the ILs effect were evaluated and rationalized based on a comparative analysis of the thermodynamic properties, enthalpies and entropies of vaporization

In situ crystallization and transformation kinetics of polymorphic forms of saturated-unsaturated-unsaturated triacylglycerols: 1-palmitoyl-2,3-dioleoyl glycerol, 1-stearoyl-2,3-dioleoyl glycerol, and 1-palmitoyl-2-oleoyl-3-linoleoyl glycerol.

Science.gov (United States)

Bayés-García, L; Calvet, T; Cuevas-Diarte, M A; Ueno, S

2016-07-01

We examined the influence of dynamic thermal treatment (variation of cooling/heating rates) on the polymorphic crystallization and transformation pathways of 1-palmitoyl-2,3-dioleoyl glycerol (POO), 1-stearoyl-2,3-dioleoyl glycerol (SOO), and 1-palmitoyl-2-oleoyl-3-linoleoyl glycerol (POL), which are major saturated-unsaturated-unsaturated (SUU) triacylglycerols (TAGs) of vegetable oils and animal fats (e.g., palm oil, olive oil, and Iberian ham fat). Using mainly a combination of differential scanning calorimetry (DSC) and synchrotron radiation X-ray diffraction (SR-XRD), we analyzed the polymorphic behavior of TAGs when high (15°Cmin -1 ), intermediate (2°Cmin -1 ), and low (0.5°Cmin -1 ) cooling and heating rates were applied. Multiple polymorphic forms were detected in POO, SOO, and POL (sub-α, α, β' 2 , and β' 1 ). Transient disordered phases, defined as kinetic liquid crystal (KLC) phases, were determined in POO and SOO for the first time. The results demonstrated that more stable forms were directly obtained from the melt by decreasing the cooling rates, whereas less stable forms predominated at high cooling rates, as confirmed in our previous work. Regarding heating rate variation, we confirmed that the nature of the polymorphic transformations observed (solid-state, transformation through KLC phase, or melt-mediation) depended largely on the heating rate. These results were discussed considering the activation energies involved in each process and compared with previous studies on TAGs with different saturated-unsaturated structures (1,3-dioleoyl-2-palmitoylglycerol, 1,3-dipalmitoyl-2-oleoyl-glycerol, trioleoyl glycerol, and 1,2-dioleoyl-3-linoleoyl glycerol). Copyright © 2016 Elsevier Ltd. All rights reserved.

Investigations on the synthesis and pharmacological properties of 4-alkoxy-2-[2-hydroxy-3-(4-aryl-1-piperazinyl)propyl]-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones.

Science.gov (United States)

Sladowska, Helena; Filipek, Barbara; Szkatuła, Dominika; Sabiniarz, Aleksandra; Kardasz, Małgorzata; Potoczek, Joanna; Sieklucka-Dziuba, Maria; Rajtar, Grazyna; Kleinrok, Zdzisław; Lis, Tadeusz

2002-11-01

Synthesis of 2-[2-hydroxy-3-(4-aryl-1-piperazinyl)propyl] derivatives of 4-alkoxy-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones (8-12) is described. The chlorides used in the above synthesis can exist in two isomeric forms: chain (18-20) and cyclic (19a, 20a). The compounds 8-12 exhibited potent analgesic activity which was superior than that of acetylsalicylic acid in two different tests. Most of the investigated imides suppressed significantly spontaneous locomotor activity in mice.

Dentritic Carbosilanes Containing Silicon-Bonded 1-[C6H2(CH2NMe2)2-3,5-Li-4] or 1-[C6H3(CH2NMe2)-4-Li-3] Mono-and Bis(amino)aryllithium End Groups: Structure of {[CH2SiMe2C6H3(CH2NMe2)-4-Li-3]2}2

NARCIS (Netherlands)

Koten, G. van; Kleij, A.W.; Kleijn, H.; Jastrzebski, J.T.B.H.; Smeets, W.J.J.; Spek, A.L.

1999-01-01

A useful synthetic procedure for the incorporation of the potentially multidentate monoanionic 1-[C6H2(CH2NMe2)2-3,5]- (=NCN) and 1-[C6H3(CH2NMe2)-4]- (=CN) ligands via the para-position on the periphery of carbosilane (CS) dendrimers has been developed. Lithiation of suitable brominated precursors

(3′R-3′-Benzyl-2′,3′-dihydro-1H-spiro[indole-3,1′-naphtho[2,3-c]pyrrole]-2,4′,9′-trione

Directory of Open Access Journals (Sweden)

Garima Sharma

2012-09-01

Full Text Available In the title compound, C26H18N2O3, the maximum deviations from planarity for the tetrahydro-1H-naphtho[2,3-c]pyrrole and indoline rings systems are 0.091 (1 and 0.012 (2 Å, respectively. These ring systems make a dihedral angle of 89.95 (6° with each other and they make dihedral angles of 73.42 (8 and 71.28 (9°, respectively, with the benzene ring. In the crystal, inversion dimers linked by pairs of N—H...O hydrogen bonds generate R22(8 loops and C—H...O interactions connect the dimers into corrugated sheets lying parallel to the bc plane.

Synthesis and structural characterization of two cobalt phosphites: 1-D (H3NC6H4NH3)Co(HPO3)2 and 2-D (NH4)2Co2(HPo3)3

International Nuclear Information System (INIS)

Cheng, C.-C.; Chang, W.-K.; Chiang, R.-K.; Wang, S.-L.

2010-01-01

Two new cobalt phosphites, (H 3 NC 6 H 4 NH 3 )Co(HPO 3 ) 2 (1) and (NH 4 ) 2 Co 2 (HPO 3 ) 3 (2), have been synthesized and characterized by single-crystal X-ray diffraction. All the cobalt atoms of 1 are in tetrahedral CoO 4 coordination. The structure of 1 comprises twisted square chains of four-rings, which contain alternating vertex-shared CoO 4 tetrahedra and HPO 3 groups. These chains are interlinked with trans-1,4-diaminocyclohexane cations by hydrogen bonds. The 2-D structure of 2 comprises anionic complex sheets with ammonium cations present between them. An anionic complex sheet contains three-deck phosphite units, which are interconnected by Co 2 O 9 to form complex layers. Magnetic susceptibility measurements of 1 and 2 showed that they have a weak antiferromagnetic interaction. - Graphical abstract: The 2-D structure of (NH 4 ) 2 Co 2 (HPO 3 ) 3 comprises anionic complex sheets with ammonium cations present between them. An anionic complex sheet contains three-deck phosphite units, which are interconnected by dimmeric Co 2 O 9 to form complex layers.

Bis[1-(3-cyanobenzylpyridinium] bis(1,2-dicyanoethene-1,2-dithiolatonickelate(II

Directory of Open Access Journals (Sweden)

Hai-Bao Duan

2011-01-01

Full Text Available In the ionic title complex, (C13H11N22[Ni(C4N2S22], the NiII ion is located on an inversion centre so the asymmetric unit contains one-half [Ni(mnt2]2− dianion (mnt2− is maleonitriledithiolate and one 1-(3-cyanobenzylpyridinium cation ([CNBzPy]+. The NiII ion in the [Ni(mnt2]2− anion is coordinated by four S atoms of two mnt2− ligands, and exhibits square-planar coordination geometry. In the [CNBzPy]+ cation, the benzene and pyridine rings are twisted with respect to the C/C/N plane incorporating the methylene C atom that links them. The crystal structure is stabilized by Coulombic interactions.

3-Carboxyquinolin-1-ium-2-carboxylate monohydrate

Directory of Open Access Journals (Sweden)

Qing Zhang

2012-03-01

Full Text Available The title compound, C11H7NO4·H2O, contains a 3-carboxyquinolin-1-ium-2-carboxylate (qda zwitterion and one water molecule. In the crystal, pairs of N—H...O hydrogen bonds link the molecules into inversion dimers, and these dimers are further connected by O—H...O hydrogen bonds into a three-dimensional supramolecular architecture. In addition, π–π interactions occur between pyridine and benzene rings from different qda ligands [centroid–centroid distance = 3.749 (1 Å] and the dihedral angles of the –CO2H and –CO2 groups to the quinoline system are 8.47 (3 and 88.16 (6°, respectively.

4-Acyloxy-2,5-diphenyl-3-oxo-2,3-dihydrothiophene 1,1-dioxides as acylating agents in the Friedel-Crafts reaction

International Nuclear Information System (INIS)

Van Ree, T.

1989-01-01

The 'activated esters', 4-acyloxy-2,5-diphenyl-3-oxo-2,3-dihydrothiophene 1,1-dioxides, easily accessible from 4,6-diphenylthieno[3,4-d][1,3]dioxol-2-one 5,5-dioxide, have been found to be excellent acylating agents in the Friedel-Crafts reaction with olefins and activated aromatic compounds. In the case of the olefins, product mixtures containing β-chloroketones were treated with 1,8-diazabicyclo[5.4.0]undex-7-ene to afford the corresponding unsaturated ketones in 30 - 73% yields, whereas aromatic ketones were obtained in high yields. The activated esters react slightly faster than the corresponding alkanoyl chlorides, and form fewer by-products

2-[4-(Methylsulfanylphenyl]naphtho[1,8-de][1,3,2]diazaborinane

Directory of Open Access Journals (Sweden)

Cathryn A. Slabber

2011-06-01

Full Text Available The title compound, C17H15BN2S, is one member in a series of diazaborinanes featuring substitution at the 1-, 2- and 3-positions in the nitrogen–boron heterocycle. The dihedral angle between the mean planes of the naphthalene and phenyl ring systems is 19.86 (6°. In the crystal structure, two C—H...π interactions link the molecules into sheets which lie parallel to the bc plane. There is a π–π interaction between each pair of centrosymmetrically related sheets [centroid–centroid distance = 3.5922 (8 Å].

High rate performance of novel cathode material Li1.33Ni1/3Co1/3Mn1/3O2 for lithium ion batteries

International Nuclear Information System (INIS)

Liu Haowen; Tan Long

2011-01-01

Highlights: → A novel cathode material with highly ordered structure has been prepared for the first time. → The charge and discharge current is 1000 mA g -1 and 2000 mA g -1 , respectively. → The results indicate better discharge capacity and cyclability. - Abstract: Li 1.33 Ni 1/3 Co 1/3 Mn 1/3 O 2 with highly ordered structure has been successfully synthesized via a simple co-precipitation process. Charge-discharge tests showed that the initial discharge capacities are 153.0 mAh g -1 and 128.9 mAh g -1 at 5 C (1000 mA g -1 ) and 10 C (2000 mA g -1 ) between 2.5 and 4.5 V, respectively. The average full-charge time of this material is less than 12 min at 5 C and 6 min at 10 C. The electrode material composed of the prepared showed a better cyclability. The excellent high rate performance is attributed to the improved ordered layered structure and the electrical conductivity. The excess Li shorten Li + diffusion distance between these submicron and nano-scaled particles. The results show that Li 1.33 Ni 1/3 Co 1/3 Mn 1/3 O 2 cathode material has potential application in lithium ion batteries.

Microwave assisted facile synthesis of {1/1,3-bis/1,3,5-tris-[(2-nitroxyethylnitramino)-2,4,6-trinitrobenzene]} using bismuth nitrate pentahydrate as an eco-friendly nitrating agent

International Nuclear Information System (INIS)

Badgujar, D.M.; Talawar, M.B.; Asthana, S.N.; Venugopalan, S.; Rao, A. Subhananda; Mahulikar, P.P.

2008-01-01

1-(2-Nitroxyethylnitramino)-2,4,6-trinitrobenzene (3a), 1,3-bis(2-nitroxyethyl nitramino)-2,4,6-trinitrobenzene (3b) and 1,3,5-tris(2-nitroxyethylnitramino)-2,4,6-trinitrobenzene (3c) were prepared by the nitration of 1-(2-hydroxyethylamino)-2,4,6-trinitrobenzene (2a) 1,3-bis(2-hydroxyethylamino)-2,4,6-trinitrobenzene (2b) and 1,3,5-tris(2-hydroxyethylamino)-2,4,6-trinitrobenzene (2c) using bismuth nitrate pentahydrate (eco-friendly nitrating agent) in tetrahydrofuran adsorbed on silica gel under microwave irradiation, respectively. Key intermediate compounds viz., 2a, 2b and 2c were synthesized by condensing picryl chloride, styphnyl chloride and 1,3,5-trichloro-2,4,6-trinitrobenzene with ethanol amine, respectively, based on the lines of the reported method. The synthesized compounds were characterized based on their physical constant, infrared (IR) spectroscopy and 1 H nuclear magnetic resonance (NMR) spectroscopy. The spectroscopic data obtained indicated the formation of nitrate esters (3a-3c). The nitration methodology adopted in the present study is of relevance in the context of green chemistry. The target compounds (3a-3c) synthesized using eco-friendly approach are of interest from the point of high energy materials (HEMs)

Cs_7Sm_1_1[TeO_3]_1_2Cl_1_6 and Rb_7Nd_1_1[TeO_3]_1_2Br_1_6, the new tellurite halides of the tetragonal Rb_6LiNd_1_1[SeO_3]_1_2Cl_1_6 structure type

International Nuclear Information System (INIS)

Charkin, Dmitri O.; Black, Cameron; Downie, Lewis J.; Sklovsky, Dmitry E.; Berdonosov, Peter S.; Olenev, Andrei V.; Zhou, Wuzong; Lightfoot, Philip; Dolgikh, Valery A.

2015-01-01

Two new rare-earth – alkali – tellurium oxide halides were synthesized by a salt flux technique and characterized by single-crystal X-ray diffraction. The structures of the new compounds Cs_7Sm_1_1[TeO_3]_1_2Cl_1_6 (I) and Rb_7Nd_1_1[TeO_3]_1_2Br_1_6 (II) (both tetragonal, space group I4/mcm) correspond to the sequence of [MLn_1_1(TeO_3)_1_2] and [M_6X_1_6] layers and bear very strong similarities to those of known selenite analogs. We discuss the trends in similarities and differences in compositions and structural details between the Se and Te compounds; more members of the family are predicted. - Graphical abstract: Two new rare-earth – alkali – tellurium oxide halides were predicted and synthesized. - Highlights: • Two new rare-earth – alkali – tellurium oxide halides were synthesized. • They adopt slab structure of rare earth-tellurium-oxygen and CsCl-like slabs. • The Br-based CsCl-like slabs have been observed first in this layered family.

Synthesis and structural study on (1E,2E,1'E,2'E)-3,3'-bis[(4-bromophenyl)-3,3'-(4-methy-1,2-phenylene diimine)] acetaldehyde dioxime: A combined experimental and theoretical study

Science.gov (United States)

Topal, T.; Kart, H. H.; Tunay Taşlı, P.; Karapınar, E.

2015-06-01

Tetradentate (1E,2E,1'E,2'E)-3,3'-bis[(4-bromophenyl)-3,3'-(4-methy-1,2-phenylene diimine)] acetaldehyde dioxime which possess N4 donor sets derived from the condensation of isonitroso- p-bromoacetophenone and 3,4-diaminotoluene are synthesized and characterized. The characterization of tetradentate Schiff base ligand has been deduced from LC-MS, FTIR, 13C and 1H NMR spectra and elemental analysis. Furthermore, the molecular geometry, infrared and NMR spectra of the title molecule in the ground state have been calculated by using the quantum chemical computational methods such as density functional theory (DFT) and ab initio Hartree-Fock (HF) methods with the 6-31G(d) and 6-311G(d) basis sets. The computed bond lengths and bond angles by using the both methods show the good agreement with each other. Moreover, the vibrational frequencies have been calculated and the scaled values have been compared with the experimental FTIR spectroscopic data. Assignments of the vibrational modes are made on the basis of potential energy distribution (PED) calculated from by using VEDA program. The correlations between the observed and calculated frequencies are in good agreement with each other as well as the correlation of the NMR data.

2-(5,6-Diphenyl-1,2,4-triazin-3-ylaniline

Directory of Open Access Journals (Sweden)

Mariusz Mojzych

2012-12-01

Full Text Available The title compound, C21H16N4, obtained under standard Suzuki cross-coupling conditions, is a model compound in the synthesis and biological activity evaluation of new aza-analogues of sildenafil containing a pyrazolo[4,3-e][1,2,4]triazine system. An N—H...N intramolecular hydrogen bond involving the aminobenzene system and the 1,2,4-triazine moiety helps to establish a near coplanar orientation of the rings with a dihedral angle of 12.04 (4°, which is believed to be necessary for the biological activity of sildenafil analogues. The 1,2,4-triazine ring is slightly distorted from planarity [r.m.s deviation = 0.0299 (11 Å] and forms dihedral angles of 58.60 (4 and 36.35 (3° with the pendant phenyl rings. The crystal packing features bifurcated N—H...(N,N hydrogen bonds linking screw-axis-related molecules into chains parallel to the [010] direction< and π–π interactions, with a centroid–centroid separation of 3.8722 (7 Å and a slippage of 1.412 (3 Å. The crystal studied was a nonmerohedral twin with a ratio of 0.707 (2:0293 (2.

Hydrogenolysis of 2-tosyloxy-1,3-propanediol into 1,3-propanediol over Raney Ni catalyst

Energy Technology Data Exchange (ETDEWEB)

Zhi, Zheng; Jianli, Wang; Zhen, Lu; Min, Luo; Miao, Zhang; Lixin, Xu; Jianbing [Zhejiang Province Key Laboratory of Biofuel, The State Key Laboratory Breeding Base of Green Chemistry-Synthesis Technology, Zhejiang University of Technology, Hangzhou (China)

2013-03-15

2-Tosyloxy-1,3-propanediol (TPD), a potential precursor for 1,3-propanediol (1,3-PD) production, is produced by the tosylation of glycerol with the help of protecting group techniques. In this work, the hydrogenolysis of TPD into 1,3-PD over Raney Ni catalyst is discussed at different reaction parameters to optimize the reaction conditions for selective formation of 1,3-PD. The mechanisms of the hydrogenolysis of TPD and the side reactions were also confirmed by gas chromatography-mass spectrometry (GC-MS) technique (author)

Multilevel Resistance Switching Memory in La2/3Ba1/3MnO3/0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3 (011) Heterostructure by Combined Straintronics-Spintronics.

Science.gov (United States)

Zhou, Weiping; Xiong, Yuanqiang; Zhang, Zhengming; Wang, Dunhui; Tan, Weishi; Cao, Qingqi; Qian, Zhenghong; Du, Youwei

2016-03-02

We demonstrate a memory device with multifield switchable multilevel states at room temperature based on the integration of straintronics and spintronics in a La2/3Ba1/3MnO3/0.7Pb(Mg1/3Nb2/3)O3-0.3PbTiO3 (PMN-PT) (011) heterostructure. By precisely controlling the electric field applied on the PMN-PT substrate, multiple nonvolatile resistance states can be generated in La2/3Ba1/3MnO3 films, which can be ascribed to the strain-modulated metal-insulator transition and phase separation of Manganite. Furthermore, because of the strong coupling between spin and charge degrees of freedom, the resistance of the La2/3Ba1/3MnO3 film can be readily modulated by magnetic field over a broad temperature range. Therefore, by combining electroresistance and magnetoresistance effects, multilevel resistance states with excellent retention and endurance properties can be achieved at room temperature with the coactions of electric and magnetic fields. The incorporation of ferroelastic strain and magnetic and resistive properties in memory cells suggests a promising approach for multistate, high-density, and low-power consumption electronic memory devices.

2,4,6-Tri-amino-1,3,5-triazin-1-ium 3-(prop-2-eno-yloxy)propano-ate acrylic acid monosolvate monohydrate.

Science.gov (United States)

Sangeetha, V; Kanagathara, N; Chakkaravarthi, G; Marchewka, M K; Anbalagan, G

2013-05-01

The asymmetric unit of the title salt, C3H7N6 (+)·C6H7O4 (-)·C3H4O2·H2O, contains a 2,4,6-tri-amino-1,3,5-triazin-1-ium cation, a 3-(prop-2-eno-yloxy)propano-ate anion and acrylic acid and water solvent mol-ecules in a 1:1:1:1 ratio and with each species in a general position. In the crystal, the components are linked into a supra-molecular layer in the bc plane via a combination of O-H⋯O, N-H⋯N and N-H⋯O hydrogen bonding. The crystal studied was a non-merohedral twin, the minor component contribution being approximately 26%.

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.

In vitro mutagenicity and genotoxicity study of 1,2-dichloroethylene, 1,1,2-trichloroethane, 1,3-dichloropropane, 1,2,3-trichloropropane and 1,1,3-trichloropropene, using the micronucleus test and the alkaline single cell gel electrophoresis technique (comet assay) in human lymphocytes.

Science.gov (United States)

Tafazoli, M; Kirsch-Volders, M

1996-12-20

The main objective of this study was to compare the cytotoxic genotoxic and mutagenic activity of a number of chlorinated aliphatic hydrocarbons, which are widely used as chemical intermediates, solvents, degreasing agents etc. in industry, and to establish the structure-toxicity relationship of the chemicals by using the most adequate determinants in estimating their toxicity. The mutagenicity and cytotoxicity of some of the candidate chemicals, namely 1,2-dichloroethylene, 1,1,2-trichloroethane, 1,3-dichloropropane, 1,2,3-trichloropropane and 1,1,3-trichloropropene were evaluated in an in vitro micronucleus assay. The cytokinesis-block methodology was applied on human lymphocytes in the presence or absence of an external metabolic activation system (S9-mix). In the micronucleus assay, all test substances, except 1,2,3-trichloropropane with and without S9-mix and 1,1,2-trichloroethane without S9-mix in the repeated experiment, exhibited a low but statistically significant mutagenic activity, compared to the concurrent control. However, none of the five chemicals was able to induce a clear and reproducible linear dose-dependent increase in micronucleus frequencies in this assay. Generally, mutagenic activity of the chemicals was found in the absence of severe cytotoxicity and/or cell cycle delay. The DNA breakage capacity and the cytotoxicity of these chemicals were also assessed in the alkaline single cell gel (SCG) electrophoresis test (comet assay) with and without S9-mix in isolated human lymphocytes. All chemical compounds induced DNA breakage, in the presence or absence of the metabolic activation system, at the doses tested. The data showed that the DNA reactivity of the chemicals increased with increasing degree of halogenation. The results of the present work suggested that the comet assay might be a more suitable and sensitive screening method than the micronucleus test for this particular class of compound. However, both assays do detect different

Synthesis of carbon-11 labeled 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinolinium derivatives as new potential PET SK{sub Ca} channel imaging agents

Energy Technology Data Exchange (ETDEWEB)

Gao Mingzhang; Wang Min [Department of Radiology, Indiana University School of Medicine, 1345 West 16th Street, L-3 Room 202, Indianapolis, IN 46202 (United States); Zheng Qihuang [Department of Radiology, Indiana University School of Medicine, 1345 West 16th Street, L-3 Room 202, Indianapolis, IN 46202 (United States)], E-mail: qzheng@iupui.edu

2008-02-15

Small conductance Ca{sup 2+}-activated K{sup +} (SK{sub Ca}) channels play an important role in many functions such as neuronal communication and behavioral plasticity, secretion, and cell proliferation. SK{sub Ca} channel modulation is associated with various brain, heart, and cancer diseases. N-methyl-laudanosine and its structurally related derivatives, substituted 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinoliniums, are reversible and selective SK{sub Ca} channel blockers. Carbon-11 labeled N-methyl-laudanosine and its tetrahydroisoquinolinium derivatives may serve as new probes for positron emission tomography (PET) to image SK{sub Ca} channels in the brain, heart, and cancer. The key intermediates, substituted isoquinolines (3a-c), were synthesized using a modification of the Pomeranz-Fritsch procedure. The precursors, substituted 1-(3,4-dimethoxybenzyl)-2-methyl-1,2,3,4-tetrahydroisoquinolines (8a-c), and their corresponding reference standards, substituted 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinoliniums (9a-c), were synthesized from compounds 3a-c with 3,4-dimethoxybenzyl chloride (2) in multiple steps with moderate to excellent chemical yields. The precursor 6,7-dimethoxy-1-(3,4-dimethoxybenzyl)-2-methyl-1,2,3, 4-tetrahydroisoquinoline (10) was commercially available, and the methylation of compound 10 with methyl iodide provided N-methyl-laudanosine (11). The target quaternary ammonium tracers, carbon-11 labeled 1-(3,4-dimethoxybenzyl)-2,2-dimethyl-1,2,3,4-tetrahydroisoquinoliniums ([{sup 11}C]9a-c and [{sup 11}C]11), were prepared by N-[{sup 11}C]methylation of the tertiary amine precursors (8a-c and 10) with [{sup 11}C]methyl triflate and isolated by a simplified solid-phase extraction (SPE) purification using a SiO{sub 2} or cation-exchange CM Sep-Pak cartridge in 40-65% radiochemical yields.

Tetraaquatetrakis{μ3-3,3′-[(E,E-ethane-1,2-diylbis(nitrilomethylidyne]benzene-1,2-diolato}octazinc(II N,N-dimethylformamide hexasolvate

Directory of Open Access Journals (Sweden)

Lan-Sun Zheng

2009-12-01

Full Text Available The asymmetric unit of the title compound [Zn8(C16H12N2O44(H2O4]·6C3H7NO, consists of eight ZnII cations, four tetravalent anionic ligands, L4− (L4− = 3,3′-(1E,1′E-(ethane-1,2-diylbis(azan-1-yl-1-ylidenebis(methan-1-yl-1-ylidenedibenzene-1,2-bis(olate, four coordinated water molecules and six N,N-dimethylformamide solvate molecules. The coordination complex comprises an octanuclear ZnII unit with its ZnII centers coordinated in two discrete distorted square-pyramidal geometries. Four ZnII atoms each coordinate to two nitrogen atoms and two phenolate oxygen atoms from an individual L4− ligand and one coordinated water molecule. The other four ZnII atoms each bind to five phenolate oxygen atoms from three different L4− ligands. In the crystal structure, the ZnII complex unit, coordinated water molecules and dimethylformamide solvate molecules are linked via O—H...O and C—H...O hydrogen bonds. Molecules are connected by additional intermolecular O—H...O and C—H...O hydrogen bonds, forming an extensive three dimensional framework.

1,2,3,3-Tetramethyl-7-nitro-3,4-dihydroisoquinolinium tetrafluoroborate

Directory of Open Access Journals (Sweden)

Mouna Bouzid

2016-04-01

Full Text Available The title salt, C13H17N2O2+·BF4−, was prepared by the methylation of the imine with Meerwein salt in dichloromethane. The asymmetric unit comprises a 1,3,3-trimethyl-7-nitro-3,4-dihydroisoquinolinium cation and a tetrafluoroborate anion. The coordination around the boron atom in the tetrafluoroborate anion is tetrahedral. The heterocyclic ring adopts a half-chair conformation. The crystal packing is governed by means of C—H...F contacts, which lead to the formation of a three-dimensional network.

Heterospin systems constructed from [Cu2Ln]3+ and [Ni(mnt)2]1-,2- Tectons: First 3p-3d-4f complexes (mnt = maleonitriledithiolato).

Science.gov (United States)

Madalan, Augustin M; Avarvari, Narcis; Fourmigué, Marc; Clérac, Rodolphe; Chibotaru, Liviu F; Clima, Sergiu; Andruh, Marius

2008-02-04

New heterospin complexes have been obtained by combining the binuclear complexes [{Cu(H(2)O)L(1)}Ln(O(2)NO)(3)] or [{CuL(2)}Ln(O(2)NO)(3)] (L(1) = N,N'-propylene-di(3-methoxysalicylideneiminato); L(2) = N,N'-ethylene-di(3-methoxysalicylideneiminato); Ln = Gd(3+), Sm(3+), Tb(3+)), with the mononuclear [CuL(1)(2)] and the nickel dithiolene complexes [Ni(mnt)(2)](q)- (q = 1, 2; mnt = maleonitriledithiolate), as follows: (1)infinity[{CuL(1)}(2)Ln(O(2)NO){Ni(mnt)(2)}].Solv.CH(3)CN (Ln = Gd(3+), Solv = CH(3)OH (1), Ln = Sm(3+), Solv = CH(3)CN (2)) and [{(CH(3)OH)CuL(2)}(2)Sm(O(2)NO)][Ni(mnt)(2)] (3) with [Ni(mnt)2]2-, [{(CH(3)CN)CuL(1)}(2)Ln(H(2)O)][Ni(mnt)(2)]3.2CH(3)CN (Ln = Gd(3+) (4), Sm(3+) (5), Tb(3+) (6)), and [{(CH(3)OH)CuL(2)}{CuL(2)}Gd(O(2)NO){Ni(mnt)(2)}][Ni(mnt)(2)].CH(2)Cl(2) (7) with [Ni(mnt))(2]*-. Trinuclear, almost linear, [CuLnCu] motifs are found in all the compounds. In the isostructural 1 and 2, two trans cyano groups from a [Ni(mnt)2]2- unit bridge two trimetallic nodes through axial coordination to the Cu centers, thus leading to the establishment of infinite chains. 3 is an ionic compound, containing discrete [{(CH(3)OH)CuL(2)}(2)Sm(O(2)NO)](2+) cations and [Ni(mnt)(2)](2-) anions. Within the series 4-6, layers of discrete [CuLnCu](3+) motifs alternate with stacks of interacting [Ni(mnt)(2)](*-) radical anions, for which two overlap modes, providing two different types of stacks, can be disclosed. The strength of the intermolecular interactions between the open-shell species is estimated through extended Hückel calculations. In compound 7, [Ni(mnt)(2)](*-) radical anions coordinate group one of the Cu centers of a trinuclear [Cu(2)Gd] motif through a CN, while discrete [Ni(mnt)(2)](*-) units are also present, overlapping in between, but also with the coordinated ones. Furthermore, the [Cu(2)Gd] moieties dimerize each other upon linkage by two nitrato groups, both acting as chelate toward the gadolinium ion from one unit and monodentate toward a

Liquid-air partition coefficients of 1,1-difluoroethane (HFC152a), 1,1,1-trifluoroethane (HFC143a), 1,1,1,2-tetrafluoroethane (HFC134a), 1,1,1,2,2-pentafluoroethane (HFC125) and 1,1,1,3,3-pentafluoropropane (HFC245fa).

Science.gov (United States)

Ernstgård, Lena; Lind, Birger; Andersen, Melvin E; Johanson, Gunnar

2010-01-01

Blood-air and tissue-blood coefficients (lambda) are essential to characterize the uptake and disposition of volatile substances, e.g. by physiologically based pharmacokinetic (PBPK) modelling. Highly volatile chemicals, including many hydrofluorocarbons (HFC) have low solubility in liquid media. These characteristics pose challenges for determining lambda values. A modified head-space vial equilibrium method was used to determine lambda values for five widely used HFCs. The method is based on automated head-space gas chromatography and injection of equal amount of chemical in two head-space vials with identical air phase volumes but different volumes of the liquid phase. The liquids used were water (physiological saline), fresh human blood, and olive oil. The average lambda values (n = 8) were as follows: 1,1-difluoroethane (HFC152a) - 1.08 (blood-air), 1.11 (water-air) and 5.6 (oil-air); 1,1,1-trifluoroethane (HFC143a) - 0.15, 0.15 and 1.90; 1,1,1,2-tetrafluoroethane (HFC134a) - 0.36, 0.35 and 3.5; 1,1,1,2,2-pentafluoroethane (HFC125) - 0.083, 0.074 and 1.71; and 1,1,1,3,3-pentafluoropropane (HFC245fa) - 0.62, 0.58 and 12.1. The lambda values appeared to be concentration-independent in the investigated range (2-200 ppm). In spite of the low lambda values, the method errors were modest, with coefficients of variation of 9, 11 and 10% for water, blood and oil, respectively.

Magnetic behavior of MnPS3 phases intercalated by [Zn2L]2+ (LH2: macrocyclic ligand obtained by condensation of 2-hydroxy-5-methyl-1,3-benzenedicarbaldehyde and 1,2-diaminobenzene)

International Nuclear Information System (INIS)

Spodine, E.; Valencia-Galvez, P.; Fuentealba, P.; Manzur, J.; Ruiz, D.; Venegas-Yazigi, D.; Paredes-Garcia, V.; Cardoso-Gil, R.; Schnelle, W.; Kniep, R.

2011-01-01

The intercalation of the cationic binuclear macrocyclic complex [Zn 2 L] 2+ (LH 2 : macrocyclic ligand obtained by the template condensation of 2-hydroxy-5-methyl-1,3-benzenedicarbaldehyde and 1,2-diaminobenzene) was achieved by a cationic exchange process, using K 0.4 Mn 0.8 PS 3 as a precursor. Three intercalated materials were obtained and characterized: (Zn 2 L) 0.05 K 0.3 Mn 0.8 PS 3 (1), (Zn 2 L) 0.1 K 0.2 Mn 0.8 PS 3 (2) and (Zn 2 L) 0.05 K 0.3 Mn 0.8 PS 3 (3), the latter phase being obtained by an assisted microwave radiation process. The magnetic data permit to estimate the Weiss temperature θ of ∼-130 K for (1); ∼-155 K for (2) and ∼-130 K for (3). The spin canting present in the potassium precursor remains unperturbed in composite (3), and spontaneous magnetization is observed under 50 K in both materials. However composites (1) and (2) do not present this spontaneous magnetization at low temperatures. The electronic properties of the intercalates do not appear to be significantly altered. The reflectance spectra of the intercalated phases (1), (2) and (3) show a gap value between 1.90 and 1.80 eV, lower than the value observed for the K 0.4 Mn 0.8 PS 3 precursor of 2.8 eV. -- Graphical Abstract: Microwave assisted synthesis was used to obtain an intercalated MnPS 3 phase with a binuclear Zn(II) macrocyclic complex. A comparative magnetic study of the composites obtained by assisted microwave and traditional synthetic methods is reported. Display Omitted Highlights: → A rapid and efficient preparation of intercalated MnPS 3 composites by assisted microwave synthesis is described. → The exchange of potassium ions of the precursor by the macrocyclic Zn(II) complex is partial. → The composite obtained by assisted microwave synthesis retains the spontaneous magnetization, observed in the low temperature range of the magnetic susceptibility of the potassium precursor. → The materials obtained by the conventional method loose the spontaneous

Novel Synthesis of 1,2,3-Triazoles via 1,3-Dipolar Cycloadditions of Alkynes to Azides in Ionic Liquid

Institute of Scientific and Technical Information of China (English)

ZHONG,Ping(钟平); GUO,Sheng-Rong(郭圣荣)

2004-01-01

2-Azido-3,5-dichloropyridine and 2-azido-5-chloro-3-fluoropyridine were given by reaction of sodium azide with 2,3,5-trichloropyridine, 3,5-dichloro-2-fluoropyridine or 5-chloro-2,3-difiuoropyridine in ionic liquids.1,3-Dipolar cycloaddition of 2-azido-3,5-dichloropyridine or 2-azido-5-chloro-3-fluoropyridine to alkynes in ionic liquids afforded the corresponding 1,4,5-trisubstituted [1,2,3]-triazoles in good yields and regioselectivities.

5-Isopropylidene-1,3-dithiolo[4,5-d][1,3]dithiole-2-thione

Directory of Open Access Journals (Sweden)

Yoshiro Yamashita

2009-05-01

Full Text Available The title compound, C7H6S5, contains a 5-ylidene-1,3-dithiolo[4,5-d][1,3]dithiole-2-thione framework, which is an important synthetic precursor of multi-dimensional organic superconductors and conductors. The molecular framework is planar with an r.m.s. deviation of 0.012 Å for the non-H atoms. In the crystal structure, molecules are linked by short intermolecular S...S interactions [3.501 (5 and 3.581 (4 Å], constructing a zigzag molecular tape network along the c axis.

Synthesis of 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2-14C and N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-YL-2-14C)acetamide

International Nuclear Information System (INIS)

Fong, M.T.; Leaffer, M.A.

1986-01-01

We have prepared the 14 C-labeled analogs of NSC 261036, 1-(2,3-dihydroxypropyl)-2-nitro-1H-imidazole-2- 14 C, and NSC 301467, N-(2-hydroxyethyl)-2-(2-nitro-1H-imidazol-1-yl-2- 14 C) acetamide, for pharmacological, drug distribution, and mechanisms of action studies. The latter is an analog designed for lower toxicity and improved properties. The former is a metabolite of, and appears to be less toxic than, misonidazole. (author)

Structure determination of two structural analogs, named 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) by synchrotron X-ray powder diffraction

Energy Technology Data Exchange (ETDEWEB)

Gündoğdu, Gülsüm; Aytaç, Sevim Peri; Müller, Melanie; Tozkoparan, Birsen; Kaynak, Filiz Betül

2017-12-01

Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C₂₃H₁₆F₂N₄S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C₂₃H₁₆ClFN₄S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space group1' mime-subtype='gif' type='simple'/>$P\\bar 1$,Z= 2, with the unit-cell parametersa= 6.37433(9),b= 11.3641(2),c= 14.09115(19) Å,α= 80.1740(8)°,β= 85.1164(8)°,γ= 80.9831(10)°,V= 991.55(3) ųof compound (1) anda= 6.53736(6),b= 11.55725(15),c= 14.01373(13) Å,α= 80.3323(7)°,β= 84.8939(6)°,γ= 79.3954(8)°,V= 1024.08(2) ųof compound (2). Structural analyses reveal that the title compounds are isostructural.

In-situ observation of domain wall motion in Pb(In{sub 1/2}Nb{sub 1/2})O{sub 3}-Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-PbTiO{sub 3} crystals

Energy Technology Data Exchange (ETDEWEB)

Lin, Dabin; Cai, Changlong [Laboratory of Thin Film Techniques and Optical Test, Xi' an Technological University, Xi' an 710032 (China); Li, Zhenrong, E-mail: zhrli@mail.xjtu.edu.cn; Li, Fei; Xu, Zhuo [Electronic Materials Research Laboratory, Key Laboratory of Education Ministry and International Center for Dielectric Research, Xi' an Jiaotong University, Xi' an 710049 (China); Zhang, Shujun, E-mail: soz1@psu.edu [Materials Research Institute, Pennsylvania State University, University Park, Pennsylvania 16802 (United States); Cheng, Yaojin [Science and Technology on Low-Light-Level Night Vision Laboratory, Xi' an 710065 (China)

2014-07-21

Various domain structures, including wave-like domains, mixed needle-like and laminar domains, typical embedded 90° and 180° domains, have been observed in unpoled rhombohedral, monoclinic, and tetragonal Pb(In{sub 1/2}Nb{sub 1/2})O{sub 3}-Pb(Mg{sub 1/3}Nb{sub 2/3})O{sub 3}-PbTiO{sub 3} (PIN-PMN-PT) crystals by polarizing light microscope; while in poled tetragonal crystals, the parallel 180° domains were reversed and only vertical 90° domain walls were observed. For 0.24PIN-0.42PMN-0.34PT crystals with morphotropic phase boundary composition, the domain wall motion was in-situ observed as a function of applied electric field along crystallographic [100] direction. With increasing the electric field from 0 to 12 kV/cm, the rhombohedral (R) domains were found to change to monoclinic (M) domains and then to tetragonal (T) domains. The electric field-induced phase transition was also confirmed by X-ray diffraction and the temperature-dependent dielectric behavior.

Antiferromagnetism at the YBa2Cu3O7/La2/3Ca1/3MnO3 interface

International Nuclear Information System (INIS)

Haberkorn, N.; Guimpel, J.; Sirena, M.; Steren, L.B.; Saldarriaga, W.; Baca, E.; Gomez, M.E.

2004-01-01

The magnetic properties of a series of YBa 2 Cu 3 O 7-x /La 2/3 Ca 1/3 MnO 3 (YBCO/LC 1/3 MO) superlattices grown by dc sputtering at high oxygen pressures (3.5 mbar) show the expected ferromagnetic behavior. However, field-cooled hysteresis loops at a low temperatures show the unexpected existence of exchange bias effect associated with the existence of ferromagnetic/antiferromagnetic (AF) interfaces. The blocking temperature (T B ) is found to be thickness dependent and the exchange bias field (H EB ) is found to be inversely proportional to the ferromagnetic layer thickness, as expected. The presence of an AF material is probably associated with interface disorder and Mn valence shift toward Mn 4+

Crystal structure of 5-{4′-[(2-{2-[2-(2-ammonioethoxyethoxy]ethoxy}ethylcarbamoyl]-4-methoxy-[1,1′-biphenyl]-3-yl}-3-oxo-1,2,5-thiadiazolidin-2-ide 1,1-dioxide: a potential inhibitor of the enzyme protein tyrosine phosphatase 1B (PTP1B

Directory of Open Access Journals (Sweden)

Kasi Viswanatharaju Ruddraraju

2015-04-01

Full Text Available The title compound, C24H32N4O8S, (I, crystallizes as a zwitterion. The terminal amine N atom of the [(2-{2-[2-(2-ammonioethoxyethoxy]ethoxy}ethylcarbamoyl] side chain is protonated, while the 1,2,5-thiadiazolidin-3-one 1,1-dioxide N atom is deprotonated. The side chain is turned over on itself with an intramolecular N—H...O hydrogen bond. The 1,2,5-thiadiazolidin-3-one 1,1-dioxide ring has an envelope conformation with the aryl-substituted N atom as the flap. Its mean plane is inclined by 62.87 (8° to the aryl ring to which it is attached, while the aryl rings of the biphenyl unit are inclined to one another by 20.81 (8°. In the crystal, molecules are linked by N—H...O and N—H...N hydrogen bonds, forming slabs lying parallel to (010. Within the slabs there are C—H...O and C—H...N hydrogen bonds and C—H...π interactions present.

Interstrand cross-linking of DNA by 1,3-bis(2-chloroethyl)-1-nitrosourea and other 1-(2-haloethyl)-1-nitrosoureas.

Science.gov (United States)

Kohn, K W

1977-05-01

Bifunctional alkylating agents are known to cross-link DNA by simultaneously alkylating two guanine residues located on opposite strands. Despite this apparent requirement for bifunctionality, 1-(2-chloroethyl)-1-nitrosoureas bearing a single alkylating function were found to cross-link DNA in vitro. Cross-linking was demonstrated by showing inhibition of alkali-induced strand separation. Extensive cross-linking was observed in DNA treated with 1-(2-chloroethyl)-1-nitrosourea, 1,3-bis-(2-chloroethyl)-1-nitrosourea, and 1-(2-chloroethyl(-3-cyclohexyl-1-nitrosourea. The reaction occurs in two steps, an intital binding followed by a second step which can proceed after removal of unbound drug. It is suggested that the first step is chloroethylation of a nucleophilic site on one strand and that the second step involves displacement of Cl- by a nucleophilic site on the opposite strand, resulting in an ethyl bridge between the strands. Consistent with this possibility, 1-(2-fluoroethyl)-3-cyclohexyl-1-nitrosourea produced much less cross-linking, as expected from the known low activity of F-, compared with Cl-, as leaving group. 1-Methyl-1-nitrosourea, which is known to depurinate DNA, produced no detectable cross-linking.

Order-disorder reactions in the ferroelectric perovskites Pb(Sc/sub 1/2/Nb/sub 1/2/)O/sub 3/ and Pb(Sc/sub 1/2/Ta/sub 1/2/)O/sub 3/. 2. Relation between ordering and properties

Energy Technology Data Exchange (ETDEWEB)

Stenger, C G.F.; Burggraaf, A J [Technische Hogeschool Twente, Enschede (Netherlands)

1980-10-16

The ordering of the trivalent and pentavalent cations in the pervoskites Pb(Sc/sub 1/2/Nb/sub 1/2/)O/sub 3/ and Pb(Sc/sub 1/2/Ta/sub 1/2/)O/sub 3/ can be varied by suitable heat treatments. The degree as well as the kind of order strongly affects the character of the FE ..-->.. PE phase transition. A spatially homogeneous disorder leads to a diffuse phase transition whereas a hybrid crystal with a nonhomogeneous disorder shows a sequence of two FE ..-->.. PE transitions.

Characterization studies of 1-(4-cyano-2-oxo-1,2-dihydro-1-pyridyl)-3-(4-cyano-1,2-dihydro-1-pyridyl) propane formed from the reaction of hydroxide Ion with 1,3-Bis-(4-cyano pyridinium)propane

International Nuclear Information System (INIS)

Fiori, Simone; Schuquel, Ivania T.A.; Meyer, Emerson; Hioka, Noboru; Silva, Idelcio N. da; Politi, Mario J.; Catalani, Luiz H.; Chaimovich, Hernan

2011-01-01

The aqueous alkaline reaction of 1,3.bis(4.cyanopyridinium)propane dibromide, a reactant constituted of two pyridinium rings linked by a three.methylene bridge, generates a novel compound, 1-(4-cyano-2-oxo-1,2-dihydro-1-pyridyl)-3-(4-cyano-1,2-dihydro-1-pyridyl) propane. The reaction pathway is attributed to the proximity of the OH. ion inserted between two pyridinium moieties, which occurs only in bis(pyridinium) derivatives connected by short methylene spacers, where charge-conformational effects are important. (author)

An intermolecular Diels-Alder cycloaddition under various condition between 1,3-cyclohexadiene and 7-oxabicyclo[2.2.1]hepta-2,5-diene-2,3-dicarboxylate

Directory of Open Access Journals (Sweden)

Özgür Yılmaz

2017-10-01

Full Text Available The reaction between 1,3-cyclohexadiene and dimethyl 7-oxabicyclo[2.2.1]hepta-2,5-diene-2,3-dicarboxylate both without a catalyst and with different catalysts, in both atmospheric and at high pressure, over 20 days were studied. At the end of the reactions, different products (retro Diels-Alder addition product 5 and Diels-Alder addition product 6 were obtained in different yields. When we look at the percentage of the addition product, it is observed that the yield of reaction at high pressure in water is the highest. All structures of these products were characterized by 1H-NMR, 13C-NMR, MS, and IR spectroscopy.

Formation and early hydration characteristics of C2.75B1.25A3$ in binary system of C2.75B1.25A3$-C2S

Directory of Open Access Journals (Sweden)

Wang, Shoude

2016-09-01

Full Text Available C2.75B1.25A3$ (2.75CaO•1.25BaO• 3Al2O3• SO3 is one of the important minerals and it govern-directly the early-strength of belite-barium calcium sulphoaluminate cement. In this paper a binary system C2.75B1.25A3$-C2S is selected to investigate the formation of C2.75B1.25A3$. In the range of 1100 °C–1200 °C, the earlier formed C2S hinders the formation of C2.75B1.25A3$. On the contrary, when the temperature is in the range of 1200 °C–1350 °C, the initially formed C2S could provide a surface for the nucleation of C2.75B1.25A3$ and cut down the potential barrier (?Gk* for the heterogeneous nucleation of C2.75B1.25A3$, which contributes to its formation. Moreover, at 1350 °C, the large amount of previously formed C2S benefits the extent of formation of C2.75B1.25A3$. The possible reason was that it could prevent sulfur evaporation. In early hydration age, AFm and AFt originating from C2.75B1.25A3$ hydration are found within 2 h and 12 h under 95% RH at 1 °C, respectively, whereas C2S is unhydrated at this moment.En el cemento de sulfoaluminato de calcio y bario, el C2.75B1.25A3$ (2.75CaO•1.25BaO• 3Al2 O3• SO3 es una de las principales fases, y regula directamente la resistencia inicial del cemento. En este trabajo, se ha seleccionado el sistema binario C2.75B1.25A3$-C2S para investigar la formación de C2.75B1.25A3$. En el rango de 1100 °C-1200 °C, el C2S formado anteriormente impide la formación de C2.75B1.25A3$, mientras que cuando la temperatura está entre 1200 °C-1350 °C, el C2S proporcionaría una superficie de nucleación de C2.75B1.25A3$ reduciendo la barrera de potencial (?Gk* para la nucleación heterogénea de C2.75B1.25A3$, lo que contribuye a su formación. Además, a 1350 °C, la gran cantidad de C2S formado beneficia la formación de C2.75B1.25A3$, ya que podía prevenir la evaporación del azufre. En las primeras etapas de la hidratación (entre 2 y 12h y 95% HR a 1 ºC se pueden encontrar AFM y AFt

2-(2,3-Dihydro-1H-indol-3-yl)ethanol

DEFF Research Database (Denmark)

Frydenvang, Karla Andrea; Sommer, Michael Bech; Heckmann, Dieter

2004-01-01

The first direct resolution of racemic 2-(2,3-dihydro-lH-indol-3-yl)ethanol-prepared by catalytic hydrogenation of 2-(lH-indol-3-yl)ethanol-has been accomplished by chiral simulated moving bed (SMB) chromatography. The single enantiomers were isolated as their dihydrogen phosphate salts. Single......-crystal X-ray analyses were successful, revealing that the (+)-enantiomer of 2-(2,3-dihydro-lH-indol-3-yl)ethanol has the (S) configuration. Chirality 16:126-130, 2004....

1,3-dialkyl- and 1,3-diaryl-3,4,5,6-tetrahydropyrimidin-2-ylidene rhodium(i) and palladium(II) complexes: synthesis, structure, and reactivity.

Science.gov (United States)

Mayr, Monika; Wurst, Klaus; Ongania, Karl-Hans; Buchmeiser, Michael R

2004-03-05

The synthesis of novel 1,3-diaryl- and 1,3-dialkylpyrimidin-2-ylidene-based N-heterocyclic carbenes (NHCs) and their rhodium(i) and palladium(II) complexes is described. The rhodium compounds bromo(cod)[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene]rhodium (7), bromo(cod)(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)rhodium (8) (cod=eta(4)-1,5-cyclooctadiene, mesityl=2,4,6-trimethylphenyl), chloro(cod)(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)rhodium (9), and chloro(cod)[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene]rhodium (10) were prepared by reaction of [[Rh(cod)Cl](2)] with lithium tert-butoxide followed by addition of 1,3-dimesityl-3,4,5,6-tetrahydropyrimidinium bromide (3), 1,3-dimesityl-3,4,5,6-tetrahydropyrimidinium tetrafluoroborate (4), 1,3-di-2-propyl-3,4,5,6-tetrahydropyrimidinium bromide (6), and 1,3-di-2-propyl-3,4,5,6-tetrahydropyrimidinium tetrafluoroborate, respectively. Complex 7 crystallizes in the monoclinic space group P2(1)/n, and 8 in the monoclinic space group P2(1). Complexes 9 and 10 were used for the synthesis of the corresponding dicarbonyl complexes dicarbonylchloro(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)rhodium (11), and dicarbonylchloro[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene]rhodium (12). The wavenumbers nu(CO I)/nu(CO II) for 11 and 12 were used as a quantitative measure for the basicity of the NHC ligand. The values of 2062/1976 and 2063/1982 cm(-1), respectively, indicate that the new NHCs are among the most basic cyclic ligands reported so far. Compounds 3 and 6 were additionally converted to the corresponding cationic silver(i) bis-NHC complexes [Ag(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2-ylidene)(2)]AgBr(2) (13) and [Ag[1,3-bis(2-propyl)-3,4,5,6-tetrahydropyrimidin-2-ylidene](2)]AgBr(2) (14), which were subsequently used in transmetalation reactions for the synthesis of the corresponding palladium(II) complexes Pd(1,3-dimesityl-3,4,5,6-tetrahydropyrimidin-2

Lithium Diffusion and Magnetism in Battery Cathode Material LixNi1/3Co1/3Mn1/3O2

International Nuclear Information System (INIS)

Månsson, M; Prša, K; Nozaki, H; Sugiyama, J; Wikberg, J M; Sassa, Y; Dahbi, M; Kamazawa, K; Sedlak, K; Watanabe, I

2014-01-01

We have studied low-temperature magnetic properties as well as high-temperature lithium ion diffusion in the battery cathode materials Li x Ni 1/3 Co 1/3 Mn 1/3 O 2 by the use of muon spin rotation/relaxation. Our data reveal that the samples enter into a 2D spin-glass state below T SG ≈ 12 K. We further show that lithium diffusion channels become active for T ≥ T diff ∼ 125 K where the Li-ion hopping-rate [v(T)] starts to increase exponentially. Further, v(T) is found to fit very well to an Arrhenius type equation and the activation energy for the diffusion process is extracted as E a ≈ 100 meV

Zn-Doped LiNi1/3Co1/3Mn1/3O2 Composite as Cathode Material for Lithium Ion Battery: Preparation, Characterization, and Electrochemical Properties

Directory of Open Access Journals (Sweden)

Han Du

2015-01-01

Full Text Available Zn-doped LiNi1/3Co1/3Mn1/3O2 composite, Li(Ni1/3Co1/3Mn1/31–xZnxO2 (x = 0.02; 0.05; 0.08, is synthesized by the sol-gel method. The crystal structure, morphology, and electrochemical performance are investigated via X-ray diffraction (XRD, scanning electron microscope (SEM, cyclic voltammetry (CV, and constant current charge/discharge experiment. The result reveals that Zn-doping cathode material can reach the initial charge/discharge capacity of 188.8/162.9 mAh·g−1 for Li(Ni1/3Co1/3Mn1/30.98Zn0.02O2 and 179.0/154.1 mAh·g−1 for Li(Ni1/3Co1/3Mn1/30.95Zn0.05O2 with the high voltage of 4.4 V at 0.1 C. Furthermore, the capacity retention of Li(Ni1/3Co1/3Mn1/30.98Zn0.02O2 is 95.1% at 0.5 C after 50 cycles at room temperature. The improved electrochemical properties of Zn-doped LiNi1/3Co1/3Mn1/3O2 are attributed to reduced electrode polarization, enhanced capacity reversibility, and excellent cyclic performance.

Synthesis of Novel Antibacterial Agents: 1-(2', 4'-Dihydroxy-5'-chlorophenyl-3-arylpropane-1, 3-Diones

Directory of Open Access Journals (Sweden)

J. I. Sheikh

2009-01-01

Full Text Available 1-(2', 4'-Dihydroxy-5'-chlorophenyl-3-arylpropane-1, 3-diones(3a-h have been synthesized by a simple and convenient method employing Baker-Venkatraman transformation on 2-aroyloxy-4-hydroxy-5-chloroacetophenones (2a-h with NaOH in dimethylsuphoxide regardless of pyridine. The structures of the synthesized compounds have been assigned on the basis of elemental and spectral analyses (IR, 1HNMR, 13C NMR, Mass. The synthesized compounds were evaluated for the antibacterial efficacy against gram negative and gram positive bacteria.

(2E-1-(4-Aminophenyl-3-(2-thienylprop-2-en-1-one ethanol hemisolvate

Directory of Open Access Journals (Sweden)

Hoong-Kun Fun

2009-10-01

Full Text Available In the title compound, C13H11NOS·0.5C2H6O, the chalcone derivative is close to planar, the dihedral angle between the thiophene and 4-aminophenyl rings being 3.1 (2°. The thiophene ring is disordered over two orientations with occupancies of 0.842 (3 and 0.158 (3. In the crystal structure, molecules are linked into chains along the b axis by N—H...O hydrogen bonds. The chains are crosslinked via N—H...π interactions involving the thiophene ring. The ethanol solvent molecule is also disordered over two positions, each with an occupancy of 0.25.

Preparation of Pb(Mg1/3Nb2/3)O3 by simultaneous precipitations

International Nuclear Information System (INIS)

Juiz, S.A.; Varela, J.A.; Santilli, C.V.; Pulcinelli, S.H.; Longo, E.

1990-01-01

Pb(Mg 1/3 Nb 2/3 )O 3 was obtained by simultaneous precipitation of Pb(NO 3 ) 2' Mg(NO 3 ) 2 . 6H 2 O and NH 4 H 2 /NbO(C 2 O 4 ) 3 ./3H 2 O in alkaline medium. DTA of the precipitates show the PMN formation between 700 and 750 0 C. XRD on powder calcined at 750 0 C indicates on other phases basiders PMN. Measurements of dielectric constants shows a Curie temperature shifted to -80 0 C. (author) [pt

Investigations of the physical and chemical properties of solid solutions Pb/Mnsub(1/2), Nbsub(1/2)/O3 - PbTiO3 - PbZrO3

International Nuclear Information System (INIS)

Szadkowska, A.; Majewska-Pilchowska, K.

1981-01-01

The preparation of the PMTZ materials on the basis of solid solutions Pb/Mnsub(1/2)/O 3 - PbTiO 3 - PbZrO 3 has been described. The X-ray analysis of the examined materials has been made, and porosity and grain size have been determined. Dielectric constant and mechanical quality factor as a function of PbZrO 3 content have been determined. The obtained results indicate that solid solutions Pb/Mnsub(1/2), Nbsub(1/2)/O 3 - PbTiO 3 - PbZrO 3 are useful piezoelectric materials. (author)

Hydrogen peroxide assisted synthesis of LiNi1/3Co1/3Mn1/3O2 as high-performance cathode for lithium-ion batteries

Science.gov (United States)

Lin, Chaohong; Zhang, Yongzhi; Chen, Li; Lei, Ying; Ou, Junke; Guo, Yong; Yuan, Hongyan; Xiao, Dan

2015-04-01

LiNi1/3Co1/3Mn1/3O2 (NCM) is a promising cathode material for lithium-ion battery. In this research, a facile co-precipitation process is employed, during which the mixed solution of NH3·H2O, H2O2 (30% aqueous solution) and LiOH·H2O is added into the nitrate solution. Notably, H2O2 is introduced as the oxidant and dispersant during the co-precipitation process to oxidize the metal ions and decrease the agglomeration of the precursor by giving out O2, and then improves the specific capacity, stability and energy density of NCM. Additionally, O3 is employed to further oxidize NCM to enhance the stability during the calcination process. The obtained NCM material with single crystal structure exhibits a high initial discharge specific capacity of 208.9 mAh g-1 at 0.1 C (1 C = 280 mA g-1), an excellent cycle stability with high retained capacity of 176.3 mAh g-1 after 50 cycles, and a high initial discharge specific capacities of 150.6 mAh g-1 at 5 C even at a high cutoff potential (4.6 V).

Ethyl 2-{4-[(1,5-dibenzyl-2,4-dioxo-2,3,4,5-tetra-hydro-1H-1,5-benzo-diazepin-3-yl)meth-yl]-1H-1,2,3-triazol-1-yl}acetate.

Science.gov (United States)

Jabli, Hind; Kandri Rodi, Y; Ladeira, Sonia; Essassi, El Mokhtar; Ng, Seik Weng

2009-12-12

The reaction of 1,5-dibenzyl-3-propargyl-1,5-benzodiazepine-2,4-dione with ethyl azido-acetate in the presence of copper sulfate pentahydrate and sodium ascorbate leads to the formation of the title regioisomer, C(30)H(29)N(5)O(4), which features a phenyl-ene ring fused with a seven-membered diazepinyl ring. The latter ring adopts a boat conformation (with the methyl-triazolylacetate-bearing C atom as the prow and the fused-ring C atoms as the stern). The benzyl groups connected to the diazepinyl ring jprotrude from the sides; the methyl-triazolylacetate substituent occupies an axial position.

2-(5-Bromo-3-isopropylsulfanyl-1-benzofuran-2-ylacetic acid

Directory of Open Access Journals (Sweden)

Pil Ja Seo

2012-01-01

Full Text Available The title compound, C13H13BrO3S, was prepared by alkaline hydrolysis of ethyl 2-(5-bromo-3-isopropylsulfanyl-1-benzofuran-2-ylacetate. In the crystal, the carboxyl groups are involved in intermolecular O—H...O hydrogen bonds, which link the molecules into dimers. These dimers are further packed into stacks along the c axis by intermolecular C—H...π interactions, and by slipped π–π interactions between the furan rings of adjacent molecules [centroid–centroid distance = 3.472 (2 Å, interplanar distance = 3.398 (2 Å and slippage = 0.713 (2 Å].

Role of alkali carbonate and salt in topochemical synthesis of K1/2Na1/2NbO3 and NaNbO3 templates

Science.gov (United States)

Lee, Jae-Seok; Jeon, Jae-Ho; Choi, Si-Young

2013-11-01

Since the properties of lead-free piezoelectric materials have thus far failed to meet those of lead-based materials, either chemical doping or morphological texturing should be employed to improve the piezoelectric properties of lead-free piezoelectric ceramics. The goal of this study was to synthesize plate-like K1/2Na1/2NbO3 and NaNbO3 particles, which are the most favorable templates for morphological texturing of K1/2Na1/2NbO3 ceramics. To achieve this goal, Bi2.5Na3.5Nb5O18 precursors in a plate-like shape were first synthesized and subsequently converted into K1/2Na1/2NbO3 or NaNbO3 particles that retain the morphology of Bi2.5Na3.5Nb5O18. In this study, we found that sodium or potassium carbonate does not play a major role in converting the Bi2.5Na3.5Nb5O18 precursor to K1/2Na1/2NbO3 or NaNbO3, on the contrary to previous reports; however, the salt contributes to the conversion reaction. All synthesis processes have been performed via a molten salt method, and scanning electron microscopy, scanning probe microscopy, and inductively coupled plasma mass spectroscopy were used to characterize the synthesized K1/2Na1/2NbO3 or NaNbO3 templates.