WorldWideScience

Sample records for reported compound synthesis

  1. Synthesis of a naphthalene-hydroxynaphthalene polymer model compound. Final report, June 13, 1990--September 12, 1991

    Energy Technology Data Exchange (ETDEWEB)

    1991-10-02

    The objective of this project was the synthesis of one pound of a new naphthalene-hydroxynaphthalene polymer model compound for use in coal combustion studies. Since this compound was an unreported compound, this effort also required the development of a synthetic route to this compound (including routes to the unique and unreported intermediates leading to its synthesis).

  2. Synthesis, Chemistry, and Applications of Heterocyclic Cage Compounds (V)

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    @@ The synthesis and chemistry of polycyclic of cage compounds have attracted considerable attention in recent years. The vast majority of the work reported in this area has dealt with carbocylic cage compounds. On the other hand, the synthesis and chemistry of heterocyclic cage compounds have received less attention. Recently, we envisioned that studies on the synthesis and chemistry of heterocyclic cage compounds can greatly expand the scopes and utilities of cage compounds.1 As part of a program that involves the synthesis, chemistry, and application of heterocyclic cage compounds, we report here the synthesis of new thia-oxa-cage compounds and the chemical nature of these thia-cages.

  3. Synthesis, Chemistry, and Applications of Heterocyclic Cage Compounds (V)

    Institute of Scientific and Technical Information of China (English)

    WU; Hsien-Jen

    2001-01-01

    The synthesis and chemistry of polycyclic of cage compounds have attracted considerable attention in recent years. The vast majority of the work reported in this area has dealt with carbocylic cage compounds. On the other hand, the synthesis and chemistry of heterocyclic cage compounds have received less attention. Recently, we envisioned that studies on the synthesis and chemistry of heterocyclic cage compounds can greatly expand the scopes and utilities of cage compounds.1 As part of a program that involves the synthesis, chemistry, and application of heterocyclic cage compounds, we report here the synthesis of new thia-oxa-cage compounds and the chemical nature of these thia-cages.  ……

  4. Tetrazolium Compounds: Synthesis and Applications in Medicine

    Directory of Open Access Journals (Sweden)

    Cheng-Xi Wei

    2015-03-01

    Full Text Available Tetrazoles represent a class of five-membered heterocyclic compounds with polynitrogen electron-rich planar structural features. This special structure makes tetrazole derivatives useful drugs, explosives, and other functional materials with a wide range of applications in many fields of medicine, agriculture, material science, etc. Based on our research works on azoles and other references in recent years, this review covers reported work on the synthesis and biological activities of tetrazole derivatives.

  5. Pyrite synthesis via polysulfide compounds

    Science.gov (United States)

    Luther, George W., III

    1991-10-01

    The reactions of Fe(II) and Fe(III) solutions with polysulfide solutions prepared from freshly synthesized Na 2S x ( x = 2, 4, 5) were studied at 25 and 100°C over the pH range 5.5 to 8. Direct and instantaneous pyrite formation was not observed in any reaction. High temperature reactions are nearly quantitative over periods of four hours with Fe(II) and polysulfide solutions. The rate of reaction at room temperature is comparable to that found by RICKARD (1975), and the observations reported here are in agreement with his mechanism of pyrite formation. Based on the polarographic results of these reactions and previous work, a refinement of the mechanism which includes dissolved iron sulfide complexes is proposed. Every reaction of equimolar amounts of polysulfide and Fe(II) gave the kinetic product "FeS" (an example of the Ostwald step rule). Polarographic results demonstrate that the "FeS" initially formed consists of (1) a complex of the form Fe(SH) + and (2) solid FeS. When excess polysulfide is present, a complex of form [Fe(SH) S x] - is present. This complex should readily allow for (1) the reduction of polysulfide by sulfide which produces S 22- in unprotonated form, and (2) the change of Fe(II) from high spin to low spin during the formation of pyrite. The reduction of polysulfide by sulfide was proposed by RICKARD (1975), but at the pH of the solutions studied herein, S 22- in solution should be protonated. The 22- ion is critical in the formation and structure of pyrite ( TOSSEL et al., 1981). The proposed complex allows for a cyclic intermediate which cleaves the reacting polysulfide to form S 22- unprotonated. As this process occurs, there is a change in the spin state of the Fe(II) from the high spin t 2g4e g2 to the low spin t 2g6 state which is an electron configuration exhibiting kinetic inertness. On change of the Fe(II) spin state, the complex irreversibly decomposes to form pyrite. The complex may be a cluster complex containing two or more

  6. Synthesis and biological evaluation of biaryl analogs of antitubulin compounds

    Energy Technology Data Exchange (ETDEWEB)

    Tozatti, Camila Santos Suniga; Khodyuk, Rejane Goncalves Diniz; Silva, Adriano Olimpio da; Santos, Edson dos Anjos dos; Amaral, Marcos Serrou do; Lima, Denis Pires de, E-mail: denis.lima@ufms.br [Centro de Ciencias Exatas e Tecnologia, Universidade Federal de Mato Grosso do Sul, Campo Grande, MS (Brazil); Hamel, Ernest [Screening Technologies Branch, Division of Cancer Treatment and Diagnosis, National Cancer Institute at Frederick, MD (United States)

    2012-07-01

    This paper reports the synthesis of methanones and esters bearing different substitution patterns as spacer groups between aromatic rings. This series of compounds can be considered phenstatin analogs. Two of the newly synthesized compounds, 5a and 5c, strongly inhibited tubulin polymerization and the binding of [{sup 3}H] colchicine to tubulin, suggesting that, akin to phenstatin and combretastatin A-4, they can bind to tubulin at the colchicine site. (author)

  7. Synthesis and biological evaluation of biaryl analogs of antitubulin compounds

    Directory of Open Access Journals (Sweden)

    Camila Santos Suniga Tozatti

    2012-01-01

    Full Text Available This paper reports the synthesis of methanones and esters bearing different substitution patterns as spacer groups between aromatic rings. This series of compounds can be considered phenstatin analogs. Two of the newly synthesized compounds, 5a and 5c, strongly inhibited tubulin polymerization and the binding of [³H] colchicine to tubulin, suggesting that, akin to phenstatin and combretastatin A-4, they can bind to tubulin at the colchicine site.

  8. Radiation synthesis of materials and compounds

    CERN Document Server

    Kharisov, Boris Ildusovich; Ortiz Méndez, Ubaldo

    2013-01-01

    Researchers and engineers working in nuclear laboratories, nuclear electric plants, and elsewhere in the radiochemical industries need a comprehensive handbook describing all possible radiation-chemistry interactions between irradiation and materials, the preparation of materials under distinct radiation types, the possibility of damage of materials under irradiation, and more. Radiation nanotechnology is still practically an undeveloped field, except for some achievements in the fabrication of metallic nanoparticles under ionizing flows. Radiation Synthesis of Materials and Compounds presents the state of the art of the synthesis of materials, composites, and chemical compounds, and describes methods based on the use of ionizing radiation. It is devoted to the preparation of various types of materials (including nanomaterials) and chemical compounds using ionizing radiation (alpha particles, beta particles, gamma rays, x-rays, and neutron, proton, and ion beams). The book presents contributions from leaders ...

  9. Synthesis of a naphthalene-hydroxynaphthalene polymer model compound

    Energy Technology Data Exchange (ETDEWEB)

    1991-10-02

    The objective of this project was the synthesis of one pound of a new naphthalene-hydroxynaphthalene polymer model compound for use in coal combustion studies. Since this compound was an unreported compound, this effort also required the development of a synthetic route to this compound (including routes to the unique and unreported intermediates leading to its synthesis).

  10. Synthesis of a new series of anti-rhinovirus compounds

    Institute of Scientific and Technical Information of China (English)

    Shi Yong Fan; Chun Lai Mi; Jun Yang; Song Li; Zhi Bing Zheng

    2007-01-01

    The synthesis of a series of 3,6-dichloropyridazine derivatives was described. In vitro experiment, all compounds exhibited an anti-rhinovirus activity, and one of the compounds 6g showed the comparable activity as our lead compound pirodavir.

  11. Synthesis of Dibenzylidene Sorbitol Series Compound

    Institute of Scientific and Technical Information of China (English)

    FENG Rongxiu; CHEN Ligong; HOU Zhongke; SONG Jian

    2007-01-01

    A series of alditol derivatives were designed and synthesized with relatively high yield. On the basis of reaction between sorbitol and a series of substituted benzaldehyde in the presence of an acid catalyst, a series of acetal derivatives were synthesized through free hydroxyl esterification. D-sorbitol acetal amido derivatives were prepared by reduction of nitryl and acylation of amino. Dsorbitol acetal carboxyl esterification derivatives were prepared through esterification and hydrolysis. By high performance liquid chromatography-mass spectra (HPLC-MS) and H nuclear magneticresonance spectra (1 H-NMR), 36 compounds prepared were identified. Among these derivatives prepared, 26 compounds have not been reported in the previous literatures.

  12. Efficient synthesis of benzothiazine and acrylamide compounds

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Ana Maria Alves; Walfrido, Simone Torres Padua; Leite, Lucia Fernanda Costa; Lima, Maria Carmo Alves; Galdino, Suely Lins; Pitta, Ivan Rocha [Universidade Federal de Pernambuco (UFPE), Recife, PE (Brazil). Dept. de Antibioticos; Barbosa Filho, Jose Maria [Universidade Federal da Paraiba (UFPB), Joao Pessoa, PB (Brazil); Simone, Carlos Alberto de; Ellena, Javier Alcides, E-mail: irpitta@gmail.co [Universidade de Sao Paulo (USP), Sao Carlos, SP (Brazil). Inst. de Fisica

    2010-07-01

    This article describes the synthesis of the new (2Z)-2-(4-methoxybenzylidene)-6-nitro-4H -benzo[1,4]thiazine-3-one, (2Z)-2-(4-methoxybenzylidene)-4-methyl-6-nitro-4H-benzo[1,4]thiazine-3-one, (2Z)-6-amino-2-(4-methoxybenzylidene)-4H -benzo[1,4]thiazine-3-one, (2Z)-6-butylamino-2-(4-methoxybenzylidene)-4-methyl-4H-benzo[1,4] -thiazine-3-one and (2E)-N-alkyl-N-(2-hydroxy-5-nitrophenyl) -3-phenylacrylamides and the spectroscopic data. The arylidenebenzothiazine compounds were prepared using the Knoevenagel condensation with substituted benzaldehydes in the presence of sodium methoxide in DMF. The presence of a nitro substituent in the 4-position, water and a slightly acid reaction medium in this condensation caused the rupture of the benzothiazine ring and subsequent formation of the phenylacrylamide compounds. A crystallographic data was presented for (2E)-3-(4-bromophenyl)-N-dodecyl-N -(2-hydroxy-5-nitrophenyl) acrylamide. (author)

  13. Synthesis and odour properties of floral smelling compounds.

    Science.gov (United States)

    Anselmi, C; Centini, M; Sega, A; Napolitano, E; Pelosi, P; Scesa, C

    1996-04-01

    Synopsis To provide further information on the relationships between chemical structure and floral odour, here we report the synthesis and the odour evaluation of some spirane derivatives, designed as conformational models of our previously described floral odorants. One of the new compounds (5-methyl-benzo[1,3]dioxole-2-spiro-1-cyclohexane), in particular, is endowed with a particularly pleasant odour of white flowers, can be easily prepared from commercial products and is more stable than other odorants of the same class; these characteristics make this odorant suitable for being used as an additive in perfumery and cosmetics.

  14. Synthesis, Properties Characterization and Applications of Various Organobismuth Compounds

    Directory of Open Access Journals (Sweden)

    Jingfei Luan

    2011-05-01

    Full Text Available Organobismuth chemistry was emphasized in this review article due to the low price, low toxicity and low radioactivity characteristics of bismuth. As an environmentally-friendly class of organometallic compounds, different types of organobismuth compounds have been used in organic synthesis, catalysis, materials, etc. The synthesis and property characterization of many organobismuth compounds had been summarized. This review article also presented a survey of various applications of organobismuth compounds in organic transformations, as reagents or catalysts. The reactivity, reaction pathways and mechanisms of reactions with organobismuths were discussed. Less common and limiting aspects of organobismuth compounds were also briefly mentioned.

  15. CARBOXYLESTERASES IN ENANTIOSELECTIVE SYNTHESIS OF ORGANIC COMPOUNDS

    Directory of Open Access Journals (Sweden)

    E. A. Shesterenko

    2013-02-01

    Full Text Available The classification, structure, and mechanism of catalytic action of carboxylesterase of different origin are presented in the review. The prospects of carboxylesterases application for metabolism and both several drugs and prodrugs activation investigation in vitro are shown. The enzyme usage as biocatalyst of stereoselective hydrolysis and synthesis of a wide range of acyclic, carbocyclic and heterocyclic compounds — esters are also urgent. It was established that enantiomers obtainable with the help of carboxylesterase are characterized by high chemical yields and optical purity; immobilization on different supports stabilizes the enzyme and allows the repeated usage of obtained biocatalysts. The own studies conducted and the enzymatic hydrolysis features of news 3-acylhydroxy-1,4-benzodiasepin-2-ones — potential anxiolytic and hypnotic means, with a help of pig liver microsomal fraction carboxylesterase have been established. For the first time the enantioselective hydrolysis of 3-acetoxy-7-bromo-1-methyl-5-phenyl-1,2-dihydro-3H-1,4-benzdiazepine-2-one was accomplished using free and immobilized in phyllophorine and alginate, stabilized by Ca2+ microsomal fraction. The S-enantiomer of substrate was isolated, which suggests the increased specificity of pig liver microsomal fraction carboxylesterase to its R-enantiomer.

  16. Synthesis of fluorinated organic compounds using oxygen difluoride

    Science.gov (United States)

    Toy, M. S.

    1971-01-01

    Oxygen difluoride synthesis is a much simpler, higher-yield procedure than reactions originally followed to synthesize various fluorinated organic compounds. Extreme care is taken in working with oxygen difluoride as its reactions present severe explosion hazard.

  17. Design and Synthesis of Novel Antileishmanial Compounds

    Directory of Open Access Journals (Sweden)

    Melanie Loedige

    2015-01-01

    Full Text Available According to the WHO, infectious diseases, and in particular neglected tropical diseases in poor developing countries, still play a significant role in a vast number of deaths reported worldwide. Among them, leishmaniasis occurs as a complex and clinically diverse illness caused by protozoan Leishmania species which are transmitted through the bite of sandflies. They develop through a complex life cycle, from promastigotes in sandflies to amastigotes in humans. The severity of disease is determined by the type of infecting Leishmania species and also depends strongly on whether the parasite infection leads to a systemic involvement or not. Since the sensitivity towards diverse medicaments highly differs among the Leishmania species, it is advantageous to treat leishmaniasis with species-specific drugs. Towards this goal we report a synthetic methodology and characterization of novel small molecular agents active against both forms of L. major. This synthetic approach allows for rapid access to new active antileishmanial drug templates and their first derivatives in moderate to very good yields. Although the compounds reported here are bioactive, the detailed biological results are part of a more comprehensive study and will be reported separately by our collaborators.

  18. Polyaromatic compounds alter placental protein synthesis in pregnant rats

    Energy Technology Data Exchange (ETDEWEB)

    Shiverick, K.T.; Ogilvie, S.; Medrano, T. (Univ. of Florida, Gainesville (United States))

    1991-03-15

    The administration of the polyaromatic compounds {beta}-naphthoflavone ({beta}NF) and 3-methylcholanthrene (3MC) to pregnant rats during mid-gestation has been shown to produce marked feto-placental growth retardation. This study examined secretory protein synthesis in placental tissue from rats following administration of {beta}NF on gestation days (gd) 11-14 or 3MC on gd 12-14. Explants of placental basal zone tissue were cultured for 24 hours in serum-free medium in the presence of ({sup 3}H)leucine. Secreted proteins were analyzed by two-dimensional SDS-polyacrylamide gel electrophoresis followed by either fluorography or immunostaining. Total incorporation of ({sup 3}H)leucine into secreted proteins was not altered in BZ explants from {beta}NF or 3MC-treated animals. However a selective decrease was observed in ({sup 3}H)leucine incorporation into a major complex of proteins with apparent molecular weight of 25-30,000 and isoelectric point between 5.3 to 5.7. This group of proteins has been further identified as being related to rat pituitary growth hormone (GH) using N-terminal amino acid microsequencing of individual spots from 2-D SDS-PA gels. This is the first report that synthesis of GH-related proteins by rat placenta is decreased following {beta}NF and 3MC administration, a change which may underlie the feto-placental growth retardation associated with these polyaromatic compounds.

  19. SYNTHESIS OF NITROGEN-CONTAINING COMPOUNDS FROM HIGHER TERPENOIDS

    Directory of Open Access Journals (Sweden)

    Aculina Aricu

    2011-06-01

    Full Text Available The presence of nitrogen in the molecule is usually accompanied either by the appearance of a new activity or the intensification of original activity characteristic for the native terpenoids. This maintains alive the scientific interest in the synthesis of such compounds. The present communication put into discussion the recently elaborated methods for preparation of the nitrogen-containing terpenic compounds.

  20. Synthesis of Intermetallic Compounds by Using Lithium Hudride

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Intermetallic compounds of AB5 type are promising materials for M-H batteries. In this report we present the results about the influence of quality of interme tallic compounds prepared by a new method of synthesis on their electrochemical pr operties. The well-known intermetallic Ln1-xMxNi5-yMe y (Ln=La, Mm; M=Zr; Me=Mn, Ge, Sn, Al, Co+Sn, Co+Ge) compounds were synthe sized by using mixtures of oxides, chlorides and carbonates of metals by intera ction with lithium hydride at 700~1000 ℃. Prepared samples have the uniform mi crostructure with average dimension of particles about 20~30 μm. Electrochemical tests show that kinetic behaviour of compositions are satisfac tory under current up to 200 mA*g-1. These compositions require practical ly no activation and limiting values of the discharge capacity were reached at 2 ~3 cycle up to 300 mAh*g-1, which can be considered as most promising f or practice.

  1. Synthesis of Novel Antifungal Triazole Compounds

    Institute of Scientific and Technical Information of China (English)

    Yong CHU; Ming Xia XU; Ding LU

    2004-01-01

    Based on our previous studies of 3D-QSAR, 38 novel objective compounds belonging to 4 series were designed and successfully synthesized directed by the idea of reconstructing the structure of non-pharmacophores while reserving essential ones in triazoles. In vitro pilot studies on their antifungal activities showed that most compounds have inhibitory effects on C.albicans and some inhibit S.cerevisiae also. The effects on C.albicans of 5 compounds are more potent than or equal to that of fluconazole or itraconazole.

  2. Synthesis and evaluation of boron compounds for neutron capture therapy of malignant brain tumors. Technical progress report No. 1, May 1, 1990--January 31, 1991

    Energy Technology Data Exchange (ETDEWEB)

    Soloway, A.H.; Barth, R.F.

    1990-12-31

    Boron neutron capture therapy offers the potentiality for treating brain tumors currently resistant to treatment. The success of this form of therapy is directly dependent upon the delivery of sufficient numbers of thermal-neutrons to tumor cells which possess high concentrations of B-10. The objective of this project is to develop chemical methodology to synthesize boron-containing compounds with the potential for becoming incorporated into rapidly-dividing malignant brain tumor cells and excluded from normal components of the brain and surrounding tissues, to develope biological methods for assessing the potential of the compound by use of cell culture or intratumoral injection, to develop analytical methodology for measuring boron in cells and tissue using direct current plasma atomic emission spectroscopy (DCP-AES) and alpha track autoradiography, to develop biochemical and HPLC procedures for evaluating compound uptake and tissue half-life, and to develop procedures required to assess both in vitro and vivo efficacy of BNCT with selected compounds.

  3. Targeting Platinum Compounds: synthesis and biological activity

    OpenAIRE

    VAN ZUTPHEN, Steven

    2005-01-01

    Inspired by cisplatin, the inorganic drug discovered by Barnett Rosenberg in 1965, the research described in this thesis uses targeting ligands, or ligands varied in a combinatorial fashion, to find platinum complexes with more specific modes of action. These studies have lead to the development of novel (solid-phase) synthetic methods and to the discovery of several compounds with promising biological properties.

  4. CAPTURED End Evaluation Synthesis Report

    NARCIS (Netherlands)

    Brouwers, J.H.A.M.

    2012-01-01

    This report provides the findings of the Synthesis Study of the CAPTURED Evaluation and is produced as part of the overall CAPTURED End Evaluation. After five years of support by the CAPTURED project the three CAPTURED partners have achieved commendable results. Ten lessons learned are formulated th

  5. Synthesis and properties of trifluoromethylating steroid compounds

    Institute of Scientific and Technical Information of China (English)

    王钟麒; 卢寿福; 张建蓉

    1997-01-01

    Trifluoromethyl steroids la,b; 2a,b; 3a,b have been synthesized by starting from estren 3,17-dicarbonyl-3,3-dimethyl ether (4) and dl-18-methyl-2(3)l5(10)-estra-diene-17-carbonyl-3-methyl ether (5),and by using trimthyltrifluoromethylsilane as the trifluoromethylating agent under the catalysis of tetrarnethylam-monium fluoride.The overall yields were 82%,76%; 54%,62%; and 27%,25%,respectively The α-configura tion of trifluoromethyl group of 17-position was determined by X-ray crystal diffraction method Compounds 1a,2a and 3a showed high affinity for rat uterus PRc.The test of biological activities of compounds 1b,2b and 3b is proceeding.

  6. Reactivity of organic compounds in catalytic synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Minachev, Kh.M.; Bragin, O.V.

    1978-01-01

    A comprehensive review of 1976 Soviet research on catalysis delivered to the 1977 annual session of the USSR Academy of Science Council on Catalysis (Baku 6/16-20/77) covers hydrocarbon reactions, including hydrogenation and hydrogenolysis, dehydrogenation, olefin dimerization and disproportionation, and cyclization and dehydrocyclization (e.g., piperylene cyclization and ethylene cyclotrimerization); catalytic and physicochemical properties of zeolites, including cracking, dehydrogenation, and hydroisomerization catalytic syntheses and conversion of heterocyclic and functional hydrocarbon derivatives, including partial and total oxidation (e.g., of o-xylene to phthalic anhydride); syntheses of thiophenes from alkanes and hydrogen sulfide over certain dehydrogenation catalysts; catalytic syntheses involving carbon oxides ( e.g., the development of a new heterogeneous catalyst for hydroformylation of olefins), and of Co-MgO zeolitic catalysts for synthesis of aliphatic hydrocarbons from carbon dioxide and hydrogen, and fabrication of high-viscosity lubricating oils over bifunctional aluminosilicate catalysts.

  7. SYNTHESIS AND CHARACTERIZATION OF NEW INTERMETALLIC COMPOUNDS

    Energy Technology Data Exchange (ETDEWEB)

    Professor Monica Sorescu

    2003-05-07

    This six-month work is focused mainly on the properties of novel magnetic intermetallics. In the first project, we synthesized several 2:17 intermetallic compounds, namely Nd{sub 2}Fe{sub 15}Si{sub 2}, Nd{sub 2}Fe{sub 15}Al{sub 2}2, Nd{sub 2}Fe{sub 15}SiAl and Nd{sub 2}Fe{sub 15}SiMn, as well as several 1:12 intermetallic compounds, such as NdFe{sub 10}Si{sub 2}, NdFe{sub 10}Al{sub 2}, NdFe{sub 10}SiAl and NdFe{sub 10}MnAl. In the second project, seven compositions of Nd{sub x}Fe{sub 100-x-y}B{sub y} ribbons were prepared by a melt spinning method with Nd and B content increasing from 7.3 and 3.6 to 11 and 6, respectively. The alloys were annealed under optimized conditions to obtain a composite material consisting of the hard magnetic Nd{sub 2}Fe{sub 14}B and soft magnetic {alpha}-Fe phases, typical of a spring magnet structure. In the third project, intermetallic compounds of the type Zr{sub 1}Cr{sub 1}Fe{sub 1}T{sub 0.8} with T=Al, Co and Fe were subjected to hydrogenation. In the fourth project, we performed three crucial experiments. In the first experiment, we subjected a mixture of Fe{sub 3}O{sub 4} and Fe(80-20 wt%) to mechanochemical activation by high-energy ball milling, for time periods ranging from 0.5 to 14 hours. In the second experiment, we ball-milled Fe{sub 3}O{sub 4}:Co{sup 2+} (x=0.1) for time intervals between 2.5 and 17.5 hours. Finally, we exposed a mixture of Fe{sub 3}O{sub 4} and Co(80-20 wt%) to mechanochemical activation for time periods ranging from 0.5 to 10 hours. In all cases, the structural and magnetic properties of the systems involved were elucidated by X-ray diffraction (XRD), Moessbauer spectroscopy and hysteresis loop measurements. The four projects resulted in four papers, which are currently being considered for publication in Intermetallics, IEEE Transactions on Magnetics, Journal of Materials Science Letters and Journal of Materials Science. The contributions reveal for the first time in literature the effect of

  8. Synthesis of Organic Compounds over Selected Types of Catalysts

    Directory of Open Access Journals (Sweden)

    Omar Mohamed Saad Ismail

    2011-05-01

    Full Text Available This study provides an overview for the utilization of different catalytic material in the synthesis of organic compounds for important reactions such as heck reaction, aldol reaction, Diels- Alder and other reactions. Comparisons between multiple catalysts for the same reaction and justifications for developing new catalyzed materials are discussed. The following topics are introduced in this work; (1 solid base catalysts, (2 clay catalysts, (3 palladium catalysts, and (4 catalysts to produce organic compound from CO2. The features of these catalysts a long with the conjugated reactions and their selectivity are explained in details, also, some alternatives for toxic or polluting catalysts used in industry are suggested.

  9. An efficient method for synthesis of organophosphorus compounds in aqueous media

    Institute of Scientific and Technical Information of China (English)

    Reza Heydari; Malek Taher Maghsoodlou; Razieh Nejat Yami

    2009-01-01

    A convenient and facile one-pot synthesis of stable phosphorus ylides and 1,4-diionic organophosphorus compounds is reported by the reaction of triphenyiphosphine, dialkylacetylenedicarboxylates and N-H, C-H or S-H acids in the presence of poly-ethyleneglycol (PEG), β-cyclodextrin (β-CD), glycerine (Gly) or ethyleneglycol (EG) in water. This methodology is of interest due to the use of water as a solvent, thus minimizing the cost operational hazards, and environmental pollution.

  10. Synthesis and Properties of Aryldicyclopentadienyltitanium(III) Compounds

    NARCIS (Netherlands)

    Teuben, J.H.; Liefde Meijer, H.J. de

    1972-01-01

    The synthesis and properties of the compounds Cp2TiR, with R=C6H5, o-, m-, p-CH3C6H4, 2,6-(CH3)2C6H3, 2,4,6-(CH3)3C6H2, C6F5, CH2C6H5, are described. Chemical and physical properties indicate that the R groups are σ-bonded to the titanium atom. The complexes are monomeric, with one unpaired electron

  11. Synthesis and anion binding properties of porphyrins and related compounds

    KAUST Repository

    Figueira, Flávio

    2016-12-02

    Over the last two decades the preparation of pyrrole-based receptors for anion recognition has attracted considerable attention. In this regard porphyrins, phthalocyanines and expanded porphyrins have been used as strong and selective receptors while the combination of those with different techniques and materials can boost their applicability in different applications as chemosensors and extracting systems. Improvements in the field, including the synthesis of this kind of compounds, can contribute to the development of efficient, cheap, and easy-to-prepare anion receptors. Extensive efforts have been made to improve the affinity and selectivity of these compounds and the continuous expansion of related research makes this chemistry even more promising. In this review, we summarize the most recent developments in anion binding studies while outlining the strategies that may be used to synthesize and functionalize these type of macrocycles. © 2016 World Scientific Publishing Company.

  12. Synthesis of hydrides by interaction of intermetallic compounds with ammonia

    Energy Technology Data Exchange (ETDEWEB)

    Tarasov, Boris P., E-mail: tarasov@icp.ac.ru [Institute of Problems of Chemical Physics of the Russian Academy of Sciences, Chernogolovka 142432 (Russian Federation); Fokin, Valentin N.; Fokina, Evelina E. [Institute of Problems of Chemical Physics of the Russian Academy of Sciences, Chernogolovka 142432 (Russian Federation); Yartys, Volodymyr A., E-mail: volodymyr.yartys@ife.no [Institute for Energy Technology, Kjeller NO 2027 (Norway); Department of Materials Science and Engineering, Norwegian University of Science and Technology, Trondheim NO 7491 (Norway)

    2015-10-05

    Highlights: • Interaction of the intermetallics A{sub 2}B, AB, AB{sub 2}, AB{sub 5} and A{sub 2}B{sub 17} with NH{sub 3} was studied. • The mechanism of interaction of the alloys with ammonia is temperature-dependent. • Hydrides, hydridonitrides, disproportionation products or metal–N–H compounds are formed. • NH{sub 4}Cl was used as an activator of the reaction between ammonia and intermetallics. • Interaction with ammonia results in the synthesis of the nanopowders. - Abstract: Interaction of intermetallic compounds with ammonia was studied as a processing route to synthesize hydrides and hydridonitrides of intermetallic compounds having various stoichiometries and types of crystal structures, including A{sub 2}B, AB, AB{sub 2}, AB{sub 5} and A{sub 2}B{sub 17} (A = Mg, Ti, Zr, Sc, Nd, Sm; B = transition metals, including Fe, Co, Ni, Ti and nontransition elements, Al and B). In presence of NH{sub 4}Cl used as an activator of the reaction between ammonia and intermetallic alloys, their interaction proceeds at rather mild P–T conditions, at temperatures 100–200 °C and at pressures of 0.6–0.8 MPa. The mechanism of interaction of the alloys with ammonia appears to be temperature-dependent and, following a rise of the interaction temperature, it leads to the formation of interstitial hydrides; interstitial hydridonitrides; disproportionation products (binary hydride; new intermetallic hydrides and binary nitrides) or new metal–nitrogen–hydrogen compounds like magnesium amide Mg(NH{sub 2}){sub 2}. The interaction results in the synthesis of the nanopowders where hydrogen and nitrogen atoms become incorporated into the crystal lattices of the intermetallic alloys. The nitrogenated materials have the smallest particle size, down to 40 nm, and a specific surface area close to 20 m{sup 2}/g.

  13. Highly Stereoselective Synthesis of a Compound Collection Based on the Bicyclic Scaffolds of Natural Products.

    Science.gov (United States)

    Annamalai, Murali; Hristeva, Stanimira; Bielska, Martyna; Ortega, Raquel; Kumar, Kamal

    2017-05-18

    Despite the great contribution of natural products in the history of successful drug discovery, there are significant limitations that persuade the pharmaceutical industry to evade natural products in drug discovery research. The extreme scarcity as well as structural complexity of natural products renders their practical synthetic access and further modifications extremely challenging. Although other alternative technologies, particularly combinatorial chemistry, were embraced by the pharmaceutical industry to get quick access to a large number of small molecules with simple frameworks that often lack three-dimensional complexity, hardly any success was achieved in the discovery of lead molecules. To acquire chemotypes beholding structural features of natural products, for instance high sp³ character, the synthesis of compound collections based on core-scaffolds of natural products presents a promising strategy. Here, we report a natural product inspired synthesis of six different chemotypes and their derivatives for drug discovery research. These bicyclic hetero- and carbocyclic scaffolds are highly novel, rich in sp³ features and with ideal physicochemical properties to display drug likeness. The functional groups on the scaffolds were exploited further to generate corresponding compound collections. Synthesis of two of these collections exemplified with ca. 350 compounds are each also presented. The whole compound library is being exposed to various biological screenings within the European Lead Factory consortium.

  14. Green chemistry approach to the synthesis of potentially bioactive aminobenzylated Mannich bases through active hydrogen compounds

    Directory of Open Access Journals (Sweden)

    S. L. VASOYA

    2005-10-01

    Full Text Available An efficient and high yield method for the synthesis of aminobenzylated Mannich bases is described. The synthesis occurs in aqueous medium at 0 ºC. The compounds show moderate antitubercular and antimicrobial activities.

  15. Synthesis and photochromic property of nanosized amino acid polyoxometalate compounds

    Science.gov (United States)

    Sun, Dehui; Zhang, Jilin; Ren, Huijuan; Cui, Zhenfeng

    2009-07-01

    A series of novel nanosized amino acid-polyoxometalate compounds were successfully synthesized using a low temperature solid-state chemical reaction method. Their compositions, structures, morphologies, photochromic properties were characterized by ICP-AES/MS, TG/DTA, FTIR, XRD, SEM and UV-Vis diffuse reflectance spectra (DRS), respectively. The elemental analysis results showed that the compounds ((HThr)7PMo12O42•4H2O, (HTyr)7PMo12O42Â.5H2O, (HSer)7PMo12O42•5H2O and (HGlu)7PMo12O42•4H2O) were obtained. The analyses of the TG/DTA, XRD and FTIR confirmed that the four compounds are new phases different from the corresponding reactants and they are composed of the polyoxometalate anions and the corresponding protonated amino acids, respectively. Observation of the SEM revealed that the particle shape (e.g. (HThr)7PMo12O42Â.4H2O nanoplates, (HTyr)7PMo12O42•5H2O nanorods, (HSer)7PMo12O42•5H2O and (HGlu)7PMo12O42•4H2O nanoparticles) depended strongly on the structures of amino acids. This implied that the amino acids can play a structural template agent role in synthesis of the Silverton-type polyoxometalate compounds. After irradiated with ultraviolet light, these samples all exhibited photochromism. Their photochromic mechanism may be explained based on Yamase's photochromic model. These photochromic compounds could be applied to the field of photosensitive materials.

  16. Synthesis and Characterization of Heteropoly Coordination Compounds Containing Optical Ligands

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    @@Introduction   The heteropolyanion phase transfer chemistry created by Pope M. T. In 1984 has opened up a new field for heteropoly compound research[1-3]. But substituting coordination water molecules by organic optically active ligand has not been reported in literatures until 1997[4].

  17. Synthesis of 1H-indazoles from N-tosylhydrazones and nitroaromatic compounds.

    Science.gov (United States)

    Liu, Zhenxing; Wang, Long; Tan, Haocheng; Zhou, Shiyi; Fu, Tianren; Xia, Ying; Zhang, Yan; Wang, Jianbo

    2014-05-21

    A new method for the synthesis of 1H-indazoles from readily available N-tosylhydrazones and nitroaromatic compounds has been developed. This transformation occurs under transition-metal-free conditions and shows a wide substrate scope. The method has been successfully applied to the formal synthesis of a bioactive compound, WAY-169916.

  18. Enzymatic synthesis of hydrophobic compounds integrated with membrane separation

    Directory of Open Access Journals (Sweden)

    Noworyta Andrzej

    2016-03-01

    Full Text Available The enzymatic synthesis of a highly hydrophobic product (dipeptide precursor in which the reaction is accompanied by the mass transfer of the reaction product to the organic phase and the substrates to the water phase is considered. Equations describing both continuous and batch processes are formulated. The range of variability in the operating parameters of such a bioreactor is specified, and the correlations reported in the literature to describe mass transfer in the membrane contactor are validated. The proposed process was verified experimentally, and good agreement between the determined and calculated concentrations was obtained in both phases.

  19. Influence of chromium compounds on microbial growth and nucleic acid synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Ogawa, Toshihiko; Usui, Masauji; Yatome, Chizuko; Idaka, Eiichi (Gifu Univ., Gifu City (Japan))

    1989-08-01

    The wastewaters of the dyeing and the tanning industry contain often various chromium compounds, e.g. K{sub 2}Cr{sub 2}O{sub 7} and CrCl{sub 3}, with a large quantity of organic substances. Biological treatments have generally been employed in these industrial factories for the biodegradation of organic substances. The toxicity of the chromium compounds have been studied regarding mutagenicity and carcinogenicity from the medical view point. This is also of interest from the view point of wastewater biological treatments. The inhibitory effects of the compounds on the cell growth and the respiration in activated sludge have been reported in detail, but mechanisms have not been sufficiently elucidated. Therefore, the influence of K{sub 2}Cr{sub 2}O{sub 7} and CrCl{sub 3} on the cell growth and on the nucleic acid content was measured. Both compounds were the inhibitors of DNA synthesis. These action resulted in increased generation time a decrease in cell division. Chromium compounds and dyes coexist often in the wastewaters of the dyeing industries. The growth inhibitions of the mixed solution were measured.

  20. Synthesis and characterization of several molybdenum chloride cluster compounds

    Energy Technology Data Exchange (ETDEWEB)

    Beers, W.W.

    1983-06-01

    Investigation into the direct synthesis of Mo/sub 4/Cl/sub 8/(P(C/sub 2/H/sub 5/)/sub 3/)/sub 4/ from Mo/sub 2/(OAc)/sub 4/ led to a synthetic procedure that produces yields greater than 80%. The single-crystal structure disclosed a planar rectangular cluster of molybdenum atoms. Metal-metal bond distances suggest that the long edges of the rectangular cluster should be considered to be single bonds and the short metal-metal bonds to be triple bonds. This view is reinforced by an extended Hueckel calculation. Attempts to add a metal atom to Mo/sub 4/Cl/sub 8/(PR/sub 3/)/sub 4/ to form Mo/sub 5/Cl/sub 10/(PR/sub 3/)/sub 3/ led instead to a compound with the composition Mo/sub 8/Cl/sub 16/(PR/sub 3/)/sub 4/. Solution and reflectance uv-visible spectra and x-ray photoelectron spectra suggest that tetranuclear molybdenum units are present. The facile reaction between Mo/sub 8/Cl/sub 16/(PR/sub 3/)/sub 4/ and PR/sub 3/ imply that the linkage between tetrameric units is weak.

  1. Allyl strontium compounds: synthesis, molecular structure and properties.

    Science.gov (United States)

    Jochmann, Phillip; Davin, Julien P; Maslek, Stefanie; Spaniol, Thomas P; Sarazin, Yann; Carpentier, Jean-Francois; Okuda, Jun

    2012-08-14

    The synthesis and attempted isolation of neutral bis(allyl)strontium [Sr(C(3)H(5))(2)] (1) resulted in the isolation of potassium tris(allyl)strontiate K[Sr(C(3)H(5))(3)] (2). In situ generated 1 shows a pronounced Brønsted basicity, inducing polymerisation of THF. Ate complex 2 crystallises as [K(THF)(2){Sr(C(3)H(5))(3)}(THF)](∞) (2·(THF)(3)). The salt-like solid state structure of 2·(THF)(3) comprises a two-dimensional network of (μ(2)-η(3):η(3)-C(3)H(5))(-) bridged potassium and strontium centres. Synthesis of allyl complexes 1 and 2 utilised SrI(2), [Sr(TMDS)(2)] (3) (TMDS = tetramethyldisilazanide), and [Sr(HMDS)(2)] (HMDS = hexamethyldisilazanide) as strontium precursors. The solid state structure of previously reported [Sr(TMDS)(2)] (3) was established by X-ray single crystal analysis as a dissymmetric dimer of [Sr(2)(TMDS)(4)(THF)(3)] (3·(THF)(3)) with multiple Si-HSr agostic interactions. The presence of ether ligands (THF, 18-crown-6) influenced the Si-HSr resonances in the NMR spectra of the amido complex 3.

  2. Possible Role of Ice in the Synthesis of Polymeric Compounds

    Science.gov (United States)

    Monnard, Pierre-Alain; Doerr, Mark; Loeffler, Philipp, M. G.

    COSPAR Session F3.6, Bremen July 18-25, 2010 Possible role of ice in the synthesis of polymeric compounds Doerr, Mark, Loeffler, Philipp M.G and Monnard, Pierre-Alain, University of Southern Den-mark, FLinT Center, Odense M, Denmark. Email: monnard@ifk.sdu.dk Cellular life relies on a collection of linear polymers (among them DNA, RNA, proteins) to perform the functions necessary to its survival. It seems likely that catalytic and informational polymers played essential roles in the emergence of the first living entities, precursors of con-temporary cells. Thus, their detection on other planetary bodies might hint at either emerging, or extant, or past life in these environments. A non-enzymatic synthesis of such polymeric materials or their precursors likely had to rely on a supply of monomers dissolved at low concentrations in an aqueous medium. An aqueous environment represents a clear hurdle to the synthesis of long polymers as it tends to inhibit polymerization due to entropic effects and favors the reverse reaction (decomposition by hy-drolysis). It was therefore proposed that polymerization could occur in a distinct micro-or nanostructured environment that would permit a local increase in the monomer concentration, reduce water activity and protect monomers and polymers from hydrolysis. Several types of micro-or nanostructured environments, among them mineral surfaces [1], lattices of organic molecules, such as amphiphile bilayer structures [2], and the eutectic phase in water-ice [3-8] have been proposed to promote RNA and peptide formation. This last environment might be of particular interest since space exploration has established that water exists on Mars, Europa, Enceladus and comets, mostly as ice. Ice deposits may also have existed on the early Earth. When an aqueous solution is cooled below its freezing point, but above the eutectic point, two aqueous phases co-exist and form the eutectic phase system: a solid (the ice crystals made of pure water

  3. Utility of Activated Nitriles in the Synthesis of Novel Heterocyclic Compounds with Antitumor Activity

    Directory of Open Access Journals (Sweden)

    Asmaa S. Salman

    2013-01-01

    Full Text Available Reaction of cyanoacetic acid hydrazide (1 with 4-methoxyacetophenone and 4-chlorobenzaldehyde (2a,b afforded the corresponding 2-cyanoacetohydrazide derivatives (3a,b respectively. The latter compounds were utilized as a key intermediate for the synthesis of new heterocyclic compounds. Newly synthesized compounds were characterized by elemental analyses and spectral data. The antitumor evaluation of some newly synthesized compounds was screened in vitro against human breast cancer cell line (MCF-7.

  4. Shock-Synthesis of Prebiotic Compounds in Impacting Simple Ices

    Science.gov (United States)

    Goldman, N.

    2013-12-01

    How and when prebiotic organic material such as amino acids appeared on the primitive planet has been debated without resolution in the open literature for close to 60 years. Earlier studies have shown that the synthesis of life-building molecules such as amino acids, polypeptides, and DNA and RNA nucleobases is much more likely in a reducing environment, e.g., rich in H2 and CH4. However, the current viewpoint is that the composition of early Earth's atmosphere was more oxidizing, consisting mainly of CO2, with significantly lesser amounts of N2, H2S, HCl, and water vapor. The possibility exists that both prebiotic raw materials and the requisite energy for their synthesis may have been delivered to the Earth simultaneously by a comet impact. Cometary ices are predominantly water, containing many small molecules important to prebiotic aqueous chemistry, e.g., NH3, CH3OH, and an impact can provide an abundant supply of energy to drive chemical reactivity. The flux of organic matter to Earth via comets and asteroids during periods of heavy bombardment may have been as high as 1013 kg/yr, delivering up to several orders of magnitude greater mass of organics than what likely pre-existed on the planet. We have conducted simulations of the chemical reactivity within impacting icy materials to close to equilibrium using quantum molecular dynamics (MD) simulations. Here, we have simulated the thermodynamic conditions of the entire impacting event, including shock compression due to impact with the planetary surface, followed by expansion due to the rarefaction wave passing through the material, and cooling and equilibration to conditions extant on the planet. Our simulations show that shock compression induces the formation of extended C-C and C-N bonded networks, which break apart to form prebiotic material upon expansion and cooling. Impacts with peak thermodynamic conditions of 36 GPa (1 GPa = 10 kbar) and 2800 K yielded functionalized aromatic hydrocarbons upon

  5. Use of Bromine and Bromo-Organic Compounds in Organic Synthesis.

    Science.gov (United States)

    Saikia, Indranirekha; Borah, Arun Jyoti; Phukan, Prodeep

    2016-06-22

    Bromination is one of the most important transformations in organic synthesis and can be carried out using bromine and many other bromo compounds. Use of molecular bromine in organic synthesis is well-known. However, due to the hazardous nature of bromine, enormous growth has been witnessed in the past several decades for the development of solid bromine carriers. This review outlines the use of bromine and different bromo-organic compounds in organic synthesis. The applications of bromine, a total of 107 bromo-organic compounds, 11 other brominating agents, and a few natural bromine sources were incorporated. The scope of these reagents for various organic transformations such as bromination, cohalogenation, oxidation, cyclization, ring-opening reactions, substitution, rearrangement, hydrolysis, catalysis, etc. has been described briefly to highlight important aspects of the bromo-organic compounds in organic synthesis.

  6. Two-temperature synthesis of non-linear optical compound CdGeAs2

    Science.gov (United States)

    Zhu, Chongqiang; Verozubova, G. A.; Mironov, Yuri P.; Lei, Zuotao; Song, Liangcheng; Ma, Tianhui; Okunev, A. O.; Yang, Chunhui

    2016-12-01

    In this work, we report on a new approach to synthesize large-scale nonlinear optical chalcopyrite compound CdGeAs2 (cadmium germanium arsenide), in which the arsenic (As) precursor and the mixture of the cadmium (Cd) and the germanium (Ge) were separated in two distinct temperature-defined zones of a furnace. Through probing the intermediate product prepared at pre-set temperature points of hot-zone area, it was revealed that the ternary compound CdGeAs2 was formed through chemical reactions among Cd3As2, CdAs2, GeAs, GeAs2 and Ge. A new intermediate crystalline compound, with determined crystal parameter c=0.9139 nm and unknown a parameter, was identified when the temperature of the mixture of Cd and Ge was set to 680 °C, which, however, disappeared when the temperature was set to 770 °C, yielding pure CdGeAs2 product. Most likely, the identified new intermediate compound has layered graphite-like structure. Moreover, we show that the described two-temperature synthesis method allows us to produce near 250 g CdGeAs2 product during one run in a horizontal furnace and 500 g in a tilted horizontal furnace with rotated reactor.

  7. Some recent work on prebiological synthesis of organic compounds.

    Science.gov (United States)

    Ponnamperuma, C.

    1966-01-01

    Origin of constituents of nucleic acid and protein molecules, noting biological molecules synthesis under conditions similar to those prevailing in prebiotic Earth, following Oparin-Haldane hypothesis

  8. Synthesis of novel ionic liquids from lignin-derived compounds

    Energy Technology Data Exchange (ETDEWEB)

    Socha, Aaron; Singh, Seema; Simmons, Blake A.; Bergeron, Maxime

    2017-09-19

    Methods and compositions are provided for synthesizing ionic liquids from lignin derived compounds comprising: contacting a starting material comprising lignin with a depolymerization agent to depolymerize the lignin and form a mixture of aldehyde containing compounds; contacting the mixture of aldehyde containing compounds with an amine under conditions suitable to convert the mixture of aldehyde containing compounds to a mixture of amine containing compounds; and contacting the mixture of amine containing compounds with an acid under conditions suitable to form an ammonium salt, thereby preparing the ionic liquid.

  9. Developmental Regimes in Africa synthesis report

    NARCIS (Netherlands)

    Booth, D.; Dietz, A.J.; Golooba-Mutebi, F.; Fuady, A.H.; Henley, D.; Kelsall, T.; Leliveld, A.H.M.; Donge, van J.K.

    2015-01-01

    Many African countries have experienced sustained economic growth, but few have achieved the type of structural change, driven by rising productivity, that has transformed mass living standards in parts of Asia. In the Developmental Regimes in Africa Synthesis Report, editor David Booth examines how

  10. Developmental Regimes in Africa synthesis report

    NARCIS (Netherlands)

    Booth, D.; Dietz, A.J.; Golooba-Mutebi, F.; Fuady, A.H.; Henley, D.; Kelsall, T.; Leliveld, A.H.M.; Donge, van J.K.

    2015-01-01

    Many African countries have experienced sustained economic growth, but few have achieved the type of structural change, driven by rising productivity, that has transformed mass living standards in parts of Asia. In the Developmental Regimes in Africa Synthesis Report, editor David Booth examines how

  11. Synthesis and evaluation of novel prenylated chalcone derivatives as anti-leishmanial and anti-trypanosomal compounds.

    Science.gov (United States)

    Passalacqua, Thais Gaban; Dutra, Luiz Antonio; de Almeida, Letícia; Velásquez, Angela Maria Arenas; Torres, Fabio Aurelio Esteves; Yamasaki, Paulo Renato; dos Santos, Mariana Bastos; Regasini, Luis Octavio; Michels, Paul A M; Bolzani, Vanderlan da Silva; Graminha, Marcia A S

    2015-08-15

    Chalcones form a class of compounds that belong to the flavonoid family and are widely distributed in plants. Their simple structure and the ease of preparation make chalcones attractive scaffolds for the synthesis of a large number of derivatives enabling the evaluation of the effects of different functional groups on biological activities. In this Letter, we report the successful synthesis of a series of novel prenylated chalcones via Claisen-Schmidt condensation and the evaluation of their effect on the viability of the Trypanosomatidae parasites Leishmania amazonensis, Leishmania infantum and Trypanosoma cruzi.

  12. Synthesis,Characterization and Biological Activities of Novel Acrylamide Compounds

    Institute of Scientific and Technical Information of China (English)

    XU Liang-zhong; XU Zhong-jie; ZHANG Gong-sheng; ZHOU Kai; ZHAI Zhi-wei

    2008-01-01

    With dimethomorph and flumorph as the leading compounds,four novel acrylamide compounds with two types of structure were designed and synthesized by means of the method of"me too chemistry".The target compounds were characterized by 1H NMR,IR,MS,and elemental analysis.The influences of solvent and raw material on the yield were investigated and optimum processing conditions were determined.The results of preliminary biological tests show that all those compounds exhibit certain antifungal activities.

  13. Synthesis and characterization of heterocyclic substituted fluoran compounds

    Directory of Open Access Journals (Sweden)

    SACHIN V. PATEL

    2007-11-01

    Full Text Available New quinazolinone-substituted fluoran compounds were synthesized by reaction of keto acid, 2’-carboxy-2-hydroxy-4-N-pyrrolidinylbenzophenone with different quinazolinone derivatives in the presence of conc. sulphuric acid. All the synthesized fluoran compounds were characterized by spectroscopic methods (IR, 1H-NMR and UV–visible spectroscopy and elemental analysis. The fluoran compounds are colourless or nearly colourless and develop colour on contact with electron-accepting compounds.

  14. Biologically Active Macrocyclic Compounds – from Natural Products to Diversity‐Oriented Synthesis

    DEFF Research Database (Denmark)

    Madsen, Charlotte Marie; Clausen, Mads Hartvig

    2011-01-01

    Macrocyclic compounds are attractive targets when searching for molecules with biological activity. The interest in this compound class is increasing, which has led to a variety of methods for tackling the difficult macrocyclization step in their synthesis. This microreview highlights some recent...

  15. Synthesis of a New Class of Highly Functionalized Phosphorus Ylides Containing Heterocyclic Compounds

    Institute of Scientific and Technical Information of China (English)

    Shaabani Ahmad; Keshipour Sajjad; Aghaei Morteza; Khodabandeh M. Hassan; Zahedi Mansour

    2012-01-01

    The zwitterionic intermediate generated from the reaction of triphenylphosphine with electron deficient acety- lenic compounds was trapped by various NH acids. The synthesis resulted in a new class of highly functionalized heterocyclic compounds. Some of the reactions produced E and Z isomers. And the stability and transformation of them were studied by dynamic 1H NMR and density functional theory (DFT) calculations.

  16. Microwave assisted synthesis of 2-pyridone and 2-pyridone based compounds

    Directory of Open Access Journals (Sweden)

    Mijin Dušan Ž.

    2014-01-01

    Full Text Available 2-Pyridones are important heterocyclic compounds that are widely used in medical chemistry, and their various derivatives have significant biological and medical applications. In this paper, the synthesis of 2-pyridones as well as 2-pyridone based compounds such as 2-quinolones using microwave assisted organic chemistry is reviewed. The review is divided in three parts. In the first part, microwave synthesis of 2-pyridones according to the type of condensation is discussed. In the second part, microwave assisted synthesis of 2-quionolones is listed. At the end of the review several examples of microwave synthesis of other 2-pyridone based compounds (ring fused N-substituted 2-pyridones are given. [Projekat Ministarstva nauke Republike Srbije, br. 172013

  17. Tanjungides A and B: New Antitumoral Bromoindole Derived Compounds from Diazona cf formosa. Isolation and Total Synthesis

    Science.gov (United States)

    Murcia, Carmen; Coello, Laura; Fernández, Rogelio; Martín, María Jesús; Reyes, Fernando; Francesch, Andrés; Munt, Simon; Cuevas, Carmen

    2014-01-01

    Tanjungides A (1) (Z isomer) and B (2) (E isomer), two novel dibrominated indole enamides, have been isolated from the tunicate Diazona cf formosa. Their structures were determined by spectroscopic methods including HRMS, and extensive 1D and 2D NMR. The stereochemistry of the cyclised cystine present in both compounds was determined by Marfey’s analysis after chemical degradation and hydrolysis. We also report the first total synthesis of these compounds using methyl 1H-indole-3-carboxylate as starting material and a linear sequence of 11 chemical steps. Tanjungides A and B exhibit significant cytotoxicity against human tumor cell lines. PMID:24566261

  18. Tanjungides A and B: new antitumoral bromoindole derived compounds from Diazona cf formosa. isolation and total synthesis.

    Science.gov (United States)

    Murcia, Carmen; Coello, Laura; Fernández, Rogelio; Martín, María Jesús; Reyes, Fernando; Francesch, Andrés; Munt, Simon; Cuevas, Carmen

    2014-02-21

    Tanjungides A (1) (Z isomer) and B (2) (E isomer), two novel dibrominated indole enamides, have been isolated from the tunicate Diazona cf formosa. Their structures were determined by spectroscopic methods including HRMS, and extensive 1D and 2D NMR. The stereochemistry of the cyclised cystine present in both compounds was determined by Marfey's analysis after chemical degradation and hydrolysis. We also report the first total synthesis of these compounds using methyl 1H-indole-3-carboxylate as starting material and a linear sequence of 11 chemical steps. Tanjungides A and B exhibit significant cytotoxicity against human tumor cell lines.

  19. Tanjungides A and B: New Antitumoral Bromoindole Derived Compounds from Diazona cf formosa. Isolation and Total Synthesis

    Directory of Open Access Journals (Sweden)

    Carmen Murcia

    2014-02-01

    Full Text Available Tanjungides A (1 (Z isomer and B (2 (E isomer, two novel dibrominated indole enamides, have been isolated from the tunicate Diazona cf formosa. Their structures were determined by spectroscopic methods including HRMS, and extensive 1D and 2D NMR. The stereochemistry of the cyclised cystine present in both compounds was determined by Marfey’s analysis after chemical degradation and hydrolysis. We also report the first total synthesis of these compounds using methyl 1H-indole-3-carboxylate as starting material and a linear sequence of 11 chemical steps. Tanjungides A and B exhibit significant cytotoxicity against human tumor cell lines.

  20. Microwave-Mediated Hetero Diels-Alder reaction: Synthesis of biologically active compounds

    OpenAIRE

    D’Aurizio, Antonio

    2009-01-01

    Heterocyclic compounds represent almost two-thirds of all the known organic compounds: they are widely distributed in nature and play a key role in a huge number of biologically important molecules including some of the most significant for human beings. A powerful tool for the synthesis of such compounds is the hetero Diels-Alder reaction (HDA), that involve a [4+2] cycloaddition reaction between heterodienes and suitable dienophiles. Among heterodienes to be used in such six-membered ...

  1. Facile Synthesis and Antimicrobial Evaluation of Some New Heterocyclic Compounds Incorporating a Biologically Active Sulfamoyl Moiety

    Directory of Open Access Journals (Sweden)

    Elham S. Darwish

    2014-01-01

    Full Text Available A facile and convenient synthesis of new heterocyclic compounds containing a sulfamoyl moiety suitable for use as antimicrobial agents was reported. The precursor 3-oxo-3-phenyl-N-(4-sulfamoylphenylpropionamide was coupled smoothly with arenediazonium salt producing hydrazones which reacted with malononitrile or triethylorthoformate affording pyridazine and triazine derivatives, respectively. Also, the reactivity of the same precursor with DMF-DMA was followed by aminotriazole; aromatic aldehydes was followed by hydrazine hydrate, triethylorthoformate, or thiourea affording triazolo[1,5-a]pyrimidine, pyrazole, acrylamide, and dihydropyrimidine derivatives, respectively. On the other hand, treatment of the precursor propionamide with phenyl isothiocyanate and KOH in DMF afforded the intermediate salt which was treated with dilute HCl followed by 2-bromo-1-phenylethanone affording carboxamide derivative. While the same intermediate salt reacted in situ with chloroacetone, ethyl 2-chloroacetate, 3-(2-bromoacetyl-2H-chromen-2-one, methyl iodide, or 2-oxo-N-phenylpropane hydrazonoyl chloride afforded the thiophene, ketene N,S-acetal, and thiadiazole derivatives, respectively. The structure of the new products was established based on elemental and spectral analysis. Antimicrobial evaluation of some selected examples from the synthesized products was carried out whereby four compounds were found to have moderate activities and one compound showed the highest activity.

  2. The reaction of diarylzinc compounds with silver salts : Synthesis and characterization of arylsilver(I) compounds

    NARCIS (Netherlands)

    Hofstee, H.K.; Boersma, J.; Kerk, G.J.M. van der

    1979-01-01

    The reaction of diarylzinc compounds with silver(I) salts is an excellent method of preparing stable arylsilver compounds in quantitative yields. These compounds have been characterized by IR and 1H and 13C NMR spectroscopy Cryoscopy in benzene shows phenylsilver to be polymeric, and the

  3. Synthesis of model compounds derived from natural clerodane insect antifeedants

    NARCIS (Netherlands)

    Klein Gebbinck, E.A.

    1999-01-01

    Insect antifeedants are compounds with the ability to reduce or inhibit insect feeding without directly killing the insect. Such compounds offer a number of properties that are highly desirable in environmentally friendly crop protection agents. Although the principle of insect control usin

  4. Synthesis and Properties of a Novel Photochromic Compound

    Institute of Scientific and Technical Information of China (English)

    Guang Fei LIU; Lang LIU; Dian Zeng JIA; Kai Bei YU

    2003-01-01

    A new photochromic compound containing pyrazolone-ring was synthesized, and its crystal structure was determined on X-ray singlecrystal diffraction, which belongs to monoclinic crystal system, space group P21/c. The UV spectrum of the compound is studied.

  5. Synthesis and Antibacterial Activity of New Cephalosporin Compounds

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Five new cephalosporin compounds were designed and synthesized, and the antibacterial activities were evaluated by the standard serial 2-fold agar dilution method in vitro.The results showed that the activities of the compounds Ⅰa and Ⅰb against ESBL E. coli and K.pneumoniae are comparable to those of Cefepime.

  6. Synthesis, structure and photoluminescent property of a novel potassic compound

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A novel 3D coordination compound of K(H2TDA)(H2O) (1) (H3TDA = 1H-1,2,3-triazole-4,5-dicarboxylic acid) has been prepared and characterized by IR spectroscopy, elemental analysis, ICP and single-crystal X-ray diffraction. Compound 1 displays strong fluorescent emission at room temperature.

  7. Synthesis and characterization of phenylethynylcarbonyl terminated novel thermosetting imide compound

    Directory of Open Access Journals (Sweden)

    H. Kimura

    2013-02-01

    Full Text Available Phenylethynyl terminated novel imide compound based on 1,3-bis(3-aminophenoxybenzene (APB and phenylethynyl trimellitic anhydride (PETA were prepared. The curing behavior of phenylethynyl terminated imide compound was investigated by differential scanning calorimetry and Fourier transform infrared spectrometry. The curing reaction of phenylethynylcarbonyl end group completed at 220°C, and proceeded much faster than that of phenylethynyl end group. Glass transition temperature of the thermosetting resin from phenylethynylcarbonyl terminated novel imide compound determined by dynamic mechanical analysis was almost the same as that of o-cresolnovolac type epoxy resin. In addition, the thermosetting resin from phenylethynylcarbonyl terminated novel imide compound exhibited excellent thermal and dimensional stabilities. These excellent properties of these phenylethynyl terminated imide compound might be due to the incorporation of alkene group or aromatic ring substitutes in the backbones, which might enhance the chain interaction (molecular packing and reduce the molecular chain mobility.

  8. [Development of novel synthetic organic reactions: synthesis of antitumor natural products and leading compounds for new pharmaceuticals].

    Science.gov (United States)

    Kita, Yasuyuki

    2002-12-01

    Biologically active natural products with unique, highly complex molecular skeletons have been used as leading compounds for raw materials of new drugs. Due to the limitations of natural supply, highly efficient, large-scale syntheses and molecular design have been sought in drug discovery. For this purpose, we have focused on a synthetic strategy effective in developing novel reactions and reagents and found several useful regio- and stereospecific reactions, contributing to the synthesis of otherwise unattainable target molecules. The application of these reactions for the total synthesis of three types of potent cytotoxic natural products for the first time is described in this paper. The basic concept is first described. Then the total synthesis of anthracyclines, fredericamycin A, and discorhabdins is reported. Novel reactions using hypervalent iodine reagents under environmentally benign conditions are also described. The future prospects for this method are discussed.

  9. Synthesis and Characterization of Coordination Compounds of Silver(I Nitrite with Ligands Ethylenethiourea and N,N'-diethylthiourea

    Directory of Open Access Journals (Sweden)

    Fariati

    2016-09-01

    Full Text Available Silver(I nitrate and ethylenethiourea (etu in 1 : 4 stochiometry have been reported [1]. Coordination compounds of A and B as silver(I nitrite with etu and silver(I nitrite with N,N’-diethylthiourea (detu respectively, have never been done. The purposes of this study are to synthesize and characterize coordination compounds of A and B. Synthesis coordination compound of A with 1 : 4, while B with 1 : 2 stoichiometry. Both of coordination compounds are conducted directly in acetonitrile. Compounds obtained are characterized by melting point, electrical conductivity measurement, SEM-EDX, qualitative nitrite test, free energy calculation and structures prediction using Spartan’14 v1.1.0. Coordination compounds of A and B are colourless needle and prism crystals; have melting point of 189°C and 103-105°C; free energy of -289,2567 and -1182.8101 kJ/mol respectively. Electrical conductivity measurement and qualitative nitrite test show that the obtained compound of A is an ionic and B is a molecular one. EDX analysis gives empirical formula prediction of two coordination compound A is C12H24AgN9O2S4 and B is C15H36AgN7O2S3.

  10. Synthesis, Characterization and Biological Activities of Organotin (IV Methylcyclohexyldithiocarbamate Compounds

    Directory of Open Access Journals (Sweden)

    Normah Awang

    2011-01-01

    Full Text Available Problem statement: The growing interest in the chemistry of sulphur donor ligands are due to their encouraging anticancer, antibacterial and antifungal activities as well as their widespread industrial application. Dithiocarbamates belong to this class and much attention has been paid to them. Approach: Novel organotin compounds with the molecular formula RmSn[S2CN(CH3(C6H11]4-m (where m = 2, R = CH3, C2H5; m = 3, R = C6H5 have been synthesized using in situ method. These compounds were characterized by elemental analysis, IR, 1H and 13C NMR spectroscopy. Results: Elemental analysis revealed that all compounds were of good purity. Infrared spectra of the compounds showed that the thioureide ν(C-N band was in the region 1450-1500 cm−1. The unsplitting band of ν(C-S in the region 974-979 cm−1 indicated the bidentate nature of the chelated dithiocarbamato legends. The 13C NMR chemical shift of the carbon atom in the N-CS2 group appeared in the range of 196.29-199.82 ppm. Single crystal analysis from one of these compounds showed that the chelating mode of the dithiocarbamate groups was isobidentate. These compounds have been screened for antibacterial activity against four bacteria; Staphylococcus aureus, Salmonella typhimurium, Pseudomonas aeruginosa and Bacillus subtilis. Only one of these compounds shows promising results against S. aureus and S. typhi. Cytotoxicity screening on human leukemic promyelocyte HL-60 cells found that two of these compounds were very active with CD50 values of 0.87 and 0.18 µg mL−1. Conclusion: The studied compounds were found to have the potential in biological activity especially in cytotoxicity where this possibly can be used for clinical trials after further research.

  11. Synthesis and Antitussive Effect of New Hydantoin Compounds

    Institute of Scientific and Technical Information of China (English)

    ZHANG Qun-li; SONG Li-jun; WANG En-si

    2013-01-01

    A series of new hydantoin compounds was synthesized with 3-bromo phenylacetic acid and 3,4-dimethylbromobenzene as starting material,7-bromo-2-tetralone and 2-bromo-5,6,8,9-tetrahydro-7-benzocycloheptenone as intermediate and Ullmann reaction,Suzuki reaction and Bucherer-Berg's reaction as key steps.The structures of the key intermediate and target compounds were confirmed by 1H NMR,13C NMR,IR and MS.Bioactivity research showed that target compounds 6a,6c,6d,6e and 15i had significant antitussive effect on the ammonia-induced cough of mice.

  12. Synthesis and Antimicrobial Activity of the Essential Oil Compounds ...

    African Journals Online (AJOL)

    NICO

    2012-08-26

    Aug 26, 2012 ... compounds was undertaken using microdilution minimum inhibitory concentration .... a Ciprofloxacin for bacteria or amphotericin B for yeasts given in µg mL–1. ... then removed under reduced pressure and the resultant oil.

  13. Synthesis of a New Series of Bone Affinity Compounds

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    A new series of bone affinity compounds were synthesized by linking chrysophanol with 5-fluorouracil derivatives. Their bone affinity was established by hydroxyapafive (HA)affinity experiment in vitro, and their cytostatic effects were shown by the MTT assay.

  14. Synthesis and Antibacterial Evaluation of Novel Heterocyclic Compounds Containing a Sulfonamido Moiety

    Directory of Open Access Journals (Sweden)

    Eman A. El-Bordany

    2013-01-01

    Full Text Available Aiming for the synthesis of new heterocyclic compounds containing a sulfonamido moiety suitable for use as antibacterial agents, the precursor ethyl {[4-N-(4,6-dimethylpyrimidin-2-ylsulfamoyl]phenylazo}cyanoacetate was reacted with a variety of active methylene compounds producing pyran, pyridine and pyridazine derivatives. Also, the reactivity of the precursor hydrazone towards hydrazine derivatives to give pyrazole and oxazole derivatives was studied. On the other hand, treatment of the same precursor with urea, thiourea and/or guanidine hydrochloride furnished pyrimidine and thiazine derivatives, respectively. The newly synthesized compounds were tested for antibacterial activity, whereby eight compounds were found to have high activities.

  15. Stereoselective total synthesis of the potent anti-asthmatic compound CMI-977 (LDP-977)

    Energy Technology Data Exchange (ETDEWEB)

    Dias, Luiz Carlos; Farina, Lui Strambi; Ferreira, Marco Antonio Barbosa, E-mail: ldias@iqm.unicamp.br [Universidade de Campinas (UNICAMP), SP (Brazil). Instituto de Quimica

    2013-02-15

    A short and efficient stereoselective total synthesis of CMI-977 (LDP-977), a potent and orally active anti-asthmatic compound, was developed. The key steps involve a highly diastereoselective Mukaiyama oxidative cyclization, which provides the trans-THF (tetrahydrofuran) unit and a Seyferth-Gilbert homologation to construct the triple bond in the target molecule. The synthesis of the key chiral building block was performed using Jacobsen hydrolytic kinetic resolution. (author)

  16. Synthesis of Heteroaromatic Compounds by Oxidative Aromatization Using an Activated Carbon/Molecular Oxygen System

    Directory of Open Access Journals (Sweden)

    Masahiko Hayashi

    2009-08-01

    Full Text Available A variety of heteroaromatic compounds, such as substituted pyridines, pyrazoles, indoles, 2-substituted imidazoles, 2-substituted imidazoles, 2-arylbenzazoles and pyrimidin-2(1H-ones are synthesized by oxidative aromatization using the activated carbon and molecular oxygen system. Mechanistic study focused on the role of activated carbon in the synthesis of 2-arylbenzazoles is also discussed. In the final section, we will disclose the efficient synthesis of substituted 9,10-anthracenes via oxidative aromatization.

  17. Synthesis and anticonvulsant activity of certain chalcone based pyrazoline compounds

    Directory of Open Access Journals (Sweden)

    Sudhakara Rao Gerapati

    2015-09-01

    Full Text Available Convulsions are involuntary, violent, spasmodic and prolonged contractions of skeletal muscles. That means a patient may have epilepsy without convulsions and vice versa. Epilepsy is a common neurological abnormality affecting about 1% of the world population. The primary objectives of these synthesized compounds are to suppress seizures and provide neuroprotection by minimizing the effects from seizure attacks. Here some of the chalcones and chalcone based various pyrazolines were evaluated for anticonvulsant activity. Their structures have been elucidated on the basis of elemental analyses and spectroscopic studies (IR, 1H-NMR & Mass spectroscopy. A preliminary evaluation of the prepared compounds has indicated that some of them exhibit moderate to significant anticonvulsant activity compared to a diazepam standard1-3.  All compounds were tested for their anticonvulsant activity using maximal electroshock induced convulsions (MES in mice at a dose level of 4 mg/kg.b.w. The compounds  Ph1, Ph2 , Py2 ,Py3 and Py4 have shown  to  good anticonvulsant activity when doses are administered as 25mg/ kg.b.w  , reduced the phases of seizures severity and  found to be active and also  increased survival rate. Remaining compounds are less efficacious.

  18. New 1,2,4-triazine bearing compounds: molecular modeling, synthesis and biotesting

    Directory of Open Access Journals (Sweden)

    Negrutska V. V.

    2009-12-01

    Full Text Available Aim. To enlarge a spectrum of biologically active compounds in the series of the 1,2,4-triazino[5,6-b] [1,4]benzothiazine (1,2,4-TBT derivatives and reveal among them efficient inhibitors of RNA synthesis Methods. The methods of structure optimization of the 3-oxo-1,2,4-TBT by fragment-oriented substitution, the molecular doking of new structures in a virtual target, the rational chemical synthesis of the theoretically predicted compounds and their testing in the system of transcription in vitro. Results. The series of 1,2,4-TBT derivatives with substituents in the benzene and triazine cycles of a base molecule were synthesized. The testing of synthesized compounds in the in vitro transcription system directed by T7 RNA polymerase revealed the structure- and concentration-dependent inhibition of the RNA synthesis by some of these compounds. The experimental and virtual screening data for all investigated compounds have a good correlation. It was found that most effective derivative is the 3-oxo-8-butyl-1,2,4-TBT which completely inhibited transcription at the concentration of 6 mg/ml. Conclusions. The biotesting results allow us to assume that the inhibition of RNA synthesis is caused by binding of the 3-oxo- 8-butyl-1,2,4-TBT to both free RNA polymerase molecules and those including in a transcriptional complex with DNA

  19. Synthesis of novel chiral compounds of purine and pyrimidine bases

    Institute of Scientific and Technical Information of China (English)

    汪毓海; 陈庆华

    1999-01-01

    The physiologically active groups such as purine and pyrimidine bases are introduced to the asymmetric ynthesis. The optically pure compounds bearing purine and pyrimidine bases (5a—5e) were prepared via the asymetric Michael addition reaction of purines and pyrimidines as Michael donators with the chiral source 5-(R)-[(1R, 2S, 5R)-menthyloxy]-2(5H)-furanone (3a), which was prepared from the natural chiral auxiliary (-)-menthol. The synthetic method was studied in detail and the new compounds were identified on the basis of their analytical data and spectroscopic data, such as [α]D20, IR, UV, 1H NMR, 13C NMR and MS. The absolute configuration of 5a was established by X-ray crystallography. The results provided an efficient synthetic route to chiral purines and pyrimidine analogues, and offered chiral sources for further research on the physiologically active compounds of chiral nucleotides.

  20. Synthesis and Assay of SIRT1-Activating Compounds.

    Science.gov (United States)

    Dai, H; Ellis, J L; Sinclair, D A; Hubbard, B P

    2016-01-01

    The NAD(+)-dependent deacetylase SIRT1 plays key roles in numerous cellular processes including DNA repair, gene transcription, cell differentiation, and metabolism. Overexpression of SIRT1 protects against a number of age-related diseases including diabetes, cancer, and Alzheimer's disease. Moreover, overexpression of SIRT1 in the murine brain extends lifespan. A number of small-molecule sirtuin-activating compounds (STACs) that increase SIRT1 activity in vitro and in cells have been developed. While the mechanism for how these compounds act on SIRT1 was once controversial, it is becoming increasingly clear that they directly interact with SIRT1 and enhance its activity through an allosteric mechanism. Here, we present detailed chemical syntheses for four STACs, each from a distinct structural class. Also, we provide a general protocol for purifying active SIRT1 enzyme and outline two complementary enzymatic assays for characterizing the effects of STACs and similar compounds on SIRT1 activity.

  1. Lanthanide alkyl and silyl compounds: Synthesis, reactivity and catalysts for green

    Energy Technology Data Exchange (ETDEWEB)

    Pindwal, Aradhana [Iowa State Univ., Ames, IA (United States)

    2016-01-01

    The last few decades have witnessed enormous research in the field of organometallic lanthanide chemistry. Our research group has developed a few rare earth alkyl compounds containing tris(dimethylsilyl)methyl ligand and explored their reactivity. This thesis focusses on extending the study of lanthanide alkyl and silyl compounds to develop strategies for their synthesis and explore their reactivity and role as catalysts in processes such as hydrosilylation and cross-dehydrocoupling.

  2. Synthesis of hetero ionic compounds using dialkylcarbonate quaternization

    Energy Technology Data Exchange (ETDEWEB)

    Friesen, Cody A.; Wolfe, Derek; Johnson, Paul Bryan

    2017-09-19

    Methods of preparing hetero ionic complexes, and ionic liquids from bisulfate salts of heteroatomic compounds using dialkylcarbonates as a primary quaternizing reactant are disclosed. Also disclosed are methods of making electrochemical cells comprising the ionic liquids, and an electrochemical cell comprising an alkaline electrolyte and a hetero ionic complex additive.

  3. Synthesis and Formation Mechanisms of Calcium Ferrite Compounds

    Institute of Scientific and Technical Information of China (English)

    Hesham I. Saleh

    2004-01-01

    Calcium ferrite compounds were prepared using calcium nitrate and iron nitrate with different molar ratios, 1:1, 0.5:1, and 1:0.5,respectively. The reactions of formation were investigated at different temperatures following the differential thermal analysis (DTA) results. Calcium ferrite compounds are CaFeO3, Ca2FeO3.5, Ca2Fe2O5, CaFe2O4, CaFe4O7, Ca7.2Fe0.8Fe30O53,Ca3Fe15O25, Ca4Fe14O25, and Ca4Fe9O17. Other reactive species of calcium nitrate are still present after firing at 450℃.Compounds were characterized using X-ray diffraction (XRD), DTA, TG, magnetic susceptibility, infrared spectra and scanning electron microscope (SEM). It is concluded that the formation mechanism of Ca-ferrite compounds depends mainly on the valency of iron cations which in role depends on its molar ratio and the existing atmosphere.

  4. Synthesis, structural and fungicidal studies of hydrazone based coordination compounds.

    Science.gov (United States)

    Sharma, Amit Kumar; Chandra, Sulekh

    2013-02-15

    The coordination compounds of the Co(II), Ni(II) and Cu(II) metal ions derived from imine based ligand, benzil bis(carbohydarzone) were structurally and pharmaceutically studied. The compounds have the general stoichiometry [M(L)]X(2) and [Co(L)X(2)], where M=Ni(II) and Cu(II), and X=NO(3)(-) and Cl(-) ions. The analytical techniques like elemental analyses, molar conductance measurements, magnetic susceptibility measurements, IR, UV/Visible, NMR, ESI mass and EPR were used to study the compounds. The key IR bands, i.e., amide I, amide II and amide III stretching vibrations accounts for the tetradentate metal binding nature of the ligand. The electronic and EPR spectral results suggest the square planar Ni(II) and Cu(II) complexes (g(iso)=2.11-2.22) and tetragonal geometry Co(II) complexes (g(iso)=2.10-2.17). To explore the compounds in the biological field, they were examined against the opportunistic pathogens, i.e., Alternaria brassicae, Aspergillus niger and Fusarium oxysporum. The partial covalent character of metal-ligand bond is supported by the orbital reduction factor k (0.62-0.92) and nephalauxetic parameter β (0.55-0.57).

  5. Ionic Liquids in the Synthesis of Antioxidant Targeted Compounds

    NARCIS (Netherlands)

    Falkeborg, Mia; Berton-Carabin, Claire C.; Cheong, Ling Zhi

    2016-01-01

    Oxidation of polyunsaturated lipids is a major cause of degradation of the sensory and nutritional quality of food products. The oxidation reactions lead to formation of volatile compounds generally associated with unpleasant flavors, which damages the sensory quality of foods. Lipid oxidation is

  6. Ionic Liquids in the Synthesis of Antioxidant Targeted Compounds

    NARCIS (Netherlands)

    Falkeborg, Mia; Berton-Carabin, Claire C.; Cheong, Ling Zhi

    2016-01-01

    Oxidation of polyunsaturated lipids is a major cause of degradation of the sensory and nutritional quality of food products. The oxidation reactions lead to formation of volatile compounds generally associated with unpleasant flavors, which damages the sensory quality of foods. Lipid oxidation is

  7. Synthesis and antiviral evaluation of bisnoradamantane sulfites and related compounds.

    Science.gov (United States)

    Valverde, Elena; Torres, Eva; Guardiola, Salvador; Naesens, Lieve; Vázquez, Santiago

    2011-03-01

    The reaction of a series of 1,2-diols with thionyl chloride led to bisnoradamantane sulfites in very good yields. The reaction has also been applied to related polycyclic scaffolds. The compounds have been tested for antiviral activity but none of them showed to be active. Several attempts to generate and trap SO from these polycyclic sulfites have been unsuccessful.

  8. Synthesis and antiviral evaluation of bisnoradamantane sulfites and related compounds

    OpenAIRE

    Valverde, Elena; Torres, Eva; Guardiola, Salvador; Naesens, Lieve; Vázquez, Santiago

    2011-01-01

    The reaction of a series of 1,2-diols with thionyl chloride led to bisnoradamantane sulfites in very good yields. The reaction has also been applied to related polycyclic scaffolds. The compounds have been tested for antiviral activity but none of them showed to be active. Several attempts to generate and trap SO from these polycyclic sulfites have been unsuccessful.

  9. Green chemistry principles in organic compound synthesis and analysis

    Directory of Open Access Journals (Sweden)

    Ruchi Verma

    2014-03-01

    Full Text Available The present review focus on various green chemistry approaches which could be utilized in the organic compounds in practical classes for undergraduate level in comparison of conventional methods. These methods avoid the usage of hazardous substances and are environmental friendly.

  10. Synthesis of mesomeric betaine compounds with imidazolium-enolate structure

    Directory of Open Access Journals (Sweden)

    Nina Gonsior

    2012-03-01

    Full Text Available The synthesis of a heterocyclic mesomeric betaine by quaternization reaction of 1-butylimidazole and tetrabromo-1,4-benzoquinone is presented. The structure was verified by means of X-ray single-crystal analysis, NMR and IR spectroscopy. Inclusion complexes of the heterocyclic mesomeric betaine with randomly methylated (1.8 β-cyclodextrin were investigated by UV–vis spectroscopy. Furthermore, the reaction conditions were applied to poly(vinylimidazole and 1,4-bis(1H-imidazol-1-ylbutane to obtain functionalized polymer networks and condensate polymers, respectively.

  11. Synthesis of a Natural Product-Like Compound Collection through Oxidative Cleavage and Cyclization of Linear Peptides

    DEFF Research Database (Denmark)

    Petersen, Rico; Le Quement, Sebastian Thordal; Nielsen, Thomas Eiland

    2014-01-01

    Massive efforts in molecular library synthesis have strived for the development of synthesis methodology which systematically delivers natural product-like compounds of high spatial complexity. Herein, we present a conceptually simple approach that builds on the power of solid-phase peptide......- ically diverse compounds was generated, and selected com- pounds were elaborated into isoform-selective metalloprotease inhibitors...

  12. Synthesis of a Natural Product-Like Compound Collection through Oxidative Cleavage and Cyclization of Linear Peptides

    DEFF Research Database (Denmark)

    Petersen, Rico; Le Quement, Sebastian Thordal; Nielsen, Thomas Eiland

    2014-01-01

    Massive efforts in molecular library synthesis have strived for the development of synthesis methodology which systematically delivers natural product-like compounds of high spatial complexity. Herein, we present a conceptually simple approach that builds on the power of solid-phase peptide......- ically diverse compounds was generated, and selected com- pounds were elaborated into isoform-selective metalloprotease inhibitors....

  13. Synthesis and Crystal Structure of a New Glycinato Copper Compound

    Institute of Scientific and Technical Information of China (English)

    XIANG Sheng-Chang; SHENG Tian-Lu; FU Rui-Biao; HU Sheng-Min; WU Xin-Tao

    2006-01-01

    A glycinato copper compound {Cu(NH2CH2COO)(H2O)ClO4} crystallizes in monoclinic, space group P21/n with a = 7.8299(9), b = 10.3807(10), c = 9.4775(12)(A), β = 109.659(6)°, V = 725.43(12)(A)3, Z = 4, Mr = 255.07, Dc = 2.335 g/cm3, F(000) = 508, μ = 3.381 mm-1, R = 0.0270 and wR = 0.0707 for 1677 observed reflections with I > 2σ(I). The title compound contains a chain in the syn-anti conformation, which is generated by the glide-plane operation. The adjacent layers made up of the chains through the connection of perchlorate are related by inversion center ope- ration, which links with each other through the hydrogen bonds.

  14. Absorption tuning of the green fluorescent protein chromophore: synthesis and studies of model compounds

    DEFF Research Database (Denmark)

    Brøndsted Nielsen, Mogens; Andersen, Lars Henrik; Rinza, Tomás Rocha

    2011-01-01

    The green fluorescent protein (GFP) chromophore is a heterocyclic compound containing a p-hydroxybenzylidine attached to an imidazol-5(4H)-one ring. This review covers the synthesis of a variety of model systems for elucidating the intrinsic optical properties of the chromophore in the gas phase...

  15. BASIC SYNTHESIS AND BIOLOGICAL ACTIVITY OF SOME PHOSPHORCONTATNING ORGANIC COMPOUNDS CONTAINING FRAGMENTS OF UREA AND TRYHLORETILAMID

    Directory of Open Access Journals (Sweden)

    Gushylyk B.

    2013-10-01

    Full Text Available Data about directions of synthesis and use of the phosphororganic compounds in technics, biology and medicine is presented in the paper. Antimicrobial activity of 51 phosphororganic salts and ilides containing urine and threechlor ethylenamide has been studied. Perspective of the development of effective antimicrobial substances has been determined

  16. Abiotic synthesis of purines and other heterocyclic compounds by the action of electrical discharges

    Science.gov (United States)

    Yuasa, S.; Flory, D.; Basile, B.; Oro, J.

    1984-01-01

    The synthesis of purines and pyrimidines using Oparin-Urey-type primitive earth atmospheres has been demonstrated by reacting methane, ethane, and ammonia in electrical discharges. Adenine, guaine, 4-aminoimidazole-5-carboxamide (AICA), and isocytosine have been identified by UV spectrometry and paper chromatography as the products of the reaction. The total yields of the identified heterocyclic compounds are 0.0023 percent. It is concluded that adenine synthesis occurs at a much lower concentration of hydrogen cyanide than has been shown by earlier studies. Pathways for the synthesis of purines from hydrogen cyanide are discussed, and a comparison of the heterocyclic compounds that have been identified in meteorites and in prebiotic reactions is presented.

  17. Synthesis of organozirconium and -hafnium compounds containing silaneopentyl-type groups

    Energy Technology Data Exchange (ETDEWEB)

    Vdovin, V.M.; Bespalova, N.B.; Ivaschenko, D.A.; Nikitin, V.S.; Sergeeva, M.B.; Strelenko, Y.A.

    1986-01-10

    This paper proposes a new method for the synthesis of organic compounds of zirconium and hafnium containing the group MCH/sub 2/Si, by reacting Zr or Hf tetrachloride with 1,1,3,3-tetramethyl-1,3-disilacyclobutane (I). Using equimolar amounts of the reactants and a temperature of 20 C, cleavage of the disilacyclobutane ring occurs with the formation of the appropriate organometallic compound 2,2,4,4-tetramethyl-4-chloro-2,4-disilabutylzirconium (or hafnium) trichloride (II). The C 13 chemical shifts of compound (II) in C/sub 6/D/sub 6/ solution relative to (CH/sub 3/)/sub 4/Si are presented.

  18. The isolation and synthesis of a novel benzofuran compound from Tephrosia purpurea, and the synthesis of several related derivatives, which suppress histamine H1 receptor gene expression.

    Science.gov (United States)

    Shill, Manik Chandra; Das, Asish Kumar; Itou, Tomohiro; Karmakar, Sanmoy; Mukherjee, Pulok K; Mizuguchi, Hiroyuki; Kashiwada, Yoshiki; Fukui, Hiroyuki; Nemoto, Hisao

    2015-11-01

    A novel naturally occurring compound with a benzofuran skeleton was isolated from a plant, Tephrosia purpurea collected in Bangladesh. The chemical synthesis of this compound confirmed its structure, and preliminary biological results showed its suppressive activity towards histamine H1 gene expression. One isomer and four derivatives were also synthesized, and their suppression activity was investigated. Although only small quantities of this compound can be isolated from its natural source, a 10 g scale synthesis was demonstrated by the newly developed method.

  19. Synthesis of Chalcone and Flavanone Compound Using Raw Material of Acetophenone and Benzaldehyde Derivative

    Directory of Open Access Journals (Sweden)

    Ismiyarto Ismiyarto

    2010-06-01

    Full Text Available Synthesis of flavanoid compounds of chalcone and flavanone groups have been conducted. Flavanoid Is one of the group natural products which is mostly found in plants and have been proved to have physiological activity as drug. In this research, chalcone proup compounds that being synthesized are: chalcone, 3,4-dimethoxychalcone, 2'-hidroxy-3,4-dimethoxychalcone where as compound of flavanone group that being synthesized is 3',4'-dimethoxyflavanone. The synthesis of chalcone group are carried out based on Claisen-Schmidt reaction by using raw material of aromatic aldehydes and aromatic ketones. The synthesis in carried out by stirring at the room temperature using alkali solution as catalyst and ethanol as solvent. The synthesis of 3',4'-dimethoxyflanone is made based on the nucleophilic 1,4 addition of the unsaturated α,β ketone. The synthesis is made by refluxing 2'-hydroxy-3,4-dimethoxychalcone in alkali condition for 12 hours. The identification of flavanoid compound is carried out by using spectroscopic IR, GC-MS and 1H-NMR methods. The result of each synthesis chalcone group are follows: chalcone as yellowish solid with m.p= 50 °C and the yield is 83.39%; 3,4-dimethoxychalcone as yellow solid with m.p= 57°C and the yield is 76.00% ; 2'-hydroxy-3,4-dimethoxychalcone as orange solid with m.p= 90 °C and the yield is 74.29%, for 3',4'-dimethoxyflavanone as pale yellow solid with m.p= 80 °C and the yield is 72.00%.

  20. Synthesis and characterization of graphite-metal fluoride intercalation compounds

    Energy Technology Data Exchange (ETDEWEB)

    McQuillan, B.W.

    1981-04-01

    The compound C/sub x/AsF/sub 5/ was prepared and characterized by x-ray diffraction and x-ray absorption, which show the presence of As(III) and As(V), and the As-F bond distances are consistent with AsF/sub 3/ and AsF/sup -//sub 6/, C/sup +//sub 8/AsF/sup -//sub 6/ and C/sup +//sub 8/OsF/sup -//sub 6/ were synthesized. The C/sub x/AsF/sub 6/ and numerous standard arsenic-flourine compounds were studied by x-ray absorption. Magnetic susceptibility of C/sup +//sub 8/OsF/sup -//sub 6/ confirms the high degree of oxidation in this compound. X-ray absorption studies were begun to determine the species present within the graphite when BrF/sub 3/ or GeF/sub 4/ + F/sub 2/ are added. In the BrF/sub 3/ case, Br/sub 2/ is evolved and only Br(III) is present in the graphite. The binary phase diagram XeF/sub 2/:Xe/sup +//sub 5/AsF/sup -//sub 6/ was investigated by melting point determination and Raman spectroscopy. This mixture near 1.3:1 forms a kinetically stable glass at room temperature and is molten at 50/sup 0/C. Several new species or phases are observed in the Raman spectra. These species have been assigned tentative structures.

  1. Amino Compounds as Inhibitors of De Novo Synthesis of Chlorobenzenes

    Science.gov (United States)

    Wang, Si-Jia; He, Pin-Jing; Lu, Wen-Tao; Shao, Li-Ming; Zhang, Hua

    2016-04-01

    The inhibitory effects of four amino compounds on the formation of chlorobenzenes (CBzs) - dioxin precursors and indicators, and the inhibitory mechanisms were explored. The results show NH4H2PO4 can decrease the total yields of CBzs (1,2di-CBz, 1,3di-CBz, 1,4di-CBz, penta-CBz and hexa-CBz) by 98.1%±1.6% and 96.1%±0.7% under air and nitrogen flow. The inhibitory effects indicated by the total yields of CBzs follow the order NH4H2PO4 > NH4HF2 > (NH4)2SO4 > NH4Br under air flow and NH4H2PO4 ≈ (NH4)2SO4 ≈ NH4HF2 >NH4Br under nitrogen flow. The inhibition mechanism revealed by thermal analysis that CuCl2 was converted to CuPO3 by reacting with NH4H2PO4 below 200 °C, which can block the transfer of chlorine and formation of C-Cl bonds at 350 °C. The effects of the other three inhibitors were weaker because their reactions with CuCl2, which form other copper compounds, and the reaction of CuCl2 with carbon, which forms C-Cl bonds, were almost simultaneous and competitive. Oxygen influenced the yield of CBzs obviously, and the total yield of five CBzs sharply increased with oxygen. Because of their high efficiency, low environmental impact, low cost, and availability, amino compounds - especially NH4H2PO4 - can be utilized as inhibitors of CBzs during incineration.

  2. Synthesis, Characterization and Biological Activities of Organotin (IV) Methylcyclohexyldithiocarbamate Compounds

    OpenAIRE

    Normah Awang; Ibrahim Baba; Yamin, Bohari M.; Mohd S. Othman; Nurul F. Kamaludin

    2011-01-01

    Problem statement: The growing interest in the chemistry of sulphur donor ligands are due to their encouraging anticancer, antibacterial and antifungal activities as well as their widespread industrial application. Dithiocarbamates belong to this class and much attention has been paid to them. Approach: Novel organotin compounds with the molecular formula RmSn[S2CN(CH3)(C6H11)]4-m (where m = 2, R = CH3, C2H5; m = 3, R = C6H5) have been synthesized using in situ method. The...

  3. Synthesis of Carbon Nanotubes and Volatile Organic Compounds Detection

    Directory of Open Access Journals (Sweden)

    Sobri S.

    2016-01-01

    Full Text Available In this work, the adsorption effect of volatile organic compounds (chloroacetophenone, acetonitrile and hexane towards the change of resistance of CNTs pellet as sensor signal was investigated. CNTs used in this research were synthesized using Floating Catalyst – Chemical Vapor Deposition (FC-CVD method in optimum condition. The synthesized CNTs were characterized using Scanning Electron Microscopy (SEM, Transmission Electron Microscopy (TEM and Raman Spectroscopy. The variation of resistance changes towards the tested gases were recorded using a multimeter. CNTs sensor pellet showed good responses towards the tested gases, however, the sensitivity, response time and recovery time of sensor pellet need to be optimized.

  4. Biological conversion of synthesis gas. Topical report: Bioreactor studies

    Energy Technology Data Exchange (ETDEWEB)

    Basu, R.; Klasson, K.T.; Clausen, E.C.; Gaddy, J.L.

    1993-09-01

    The purpose of the proposed research is to develop a technically and economically feasible process for biologically producing H{sub 2} from synthesis gas while, at the same time, removing harmful sulfur gas compounds. Six major tasks are being studied: culture development, where the best cultures are selected and conditions optimized for simultaneous hydrogen production and sulfur gas removal; mass transfer and kinetic studies in which equations necessary for process design are developed; bioreactor design studies, where the cultures chosen in Task 1 are utilized in continuous reaction vessels to demonstrate process feasibility and define operating conditions; evaluation of biological synthesis gas conversion under limiting conditions in preparation for industrial demonstration studies; process scale-up where laboratory data are scaled to larger-size units in preparation for process demonstration in a pilot-scale unit; and economic evaluation, where process simulations are used to project process economics and identify high cost areas during sensitivity analyses. The purpose of this report is to present results from bioreactor studies involving H{sub 2} production by water gas shift and H{sub 2}S removal to produce elemental sulfur. Many of the results for H{sub 2} production by Rhodospirillum rubrum have been presented during earlier contracts. Thus, this report concentrates mainly on H{sub 2}S conversion to elemental sulfur by R. rubrum.

  5. Synthesis of 6-phosphofructose aspartic acid and some related Amadori compounds.

    Science.gov (United States)

    Hansen, Alexandar L; Behrman, Edward J

    2016-08-05

    We describe the synthesis and characterization of 6-phosphofructose-aspartic acid, an intermediate in the metabolism of fructose-asparagine by Salmonella. We also report improved syntheses of fructose-asparagine itself and of fructose-aspartic acid.

  6. Synthesis, Characterization and Properties of Nanoparticles of Intermetallic Compounds

    Energy Technology Data Exchange (ETDEWEB)

    DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States)

    2015-03-12

    The research program from 2010 to the end of the grant focused on understanding the factors important to the synthesis of single phase intermetallic nano-particles (NPs), their size, crystalline order, surface properties and electrochemical activity. The synthetic method developed is a co-reduction of mixtures of single metal precursors by strong, soluble reducing agents in a non-protic solvent, tetrahydrofuran (THF). With some exceptions, the particles obtained by room temperature reduction are random alloys that need to be annealed at modest temperatures (200 to 600 °C) in order to develop an ordered structure. To avoid significant particle size growth and agglomeration, the particles must be protected by surface coatings. We developed a novel method of coating the metal nanoparticles with KCl, a by-product of the reduction reaction if the proper reducing agents are employed. In that case, a composite product containing individual metal nanoparticles in a KCl matrix is obtained. The composite can be heated to at least 600 °C without significant agglomeration or growth in particle size. Washing the annealed product in the presence of catalyst supports in ethylene glycol removes the KCl and deposits the particles on the support. Six publications present the method and its application to producing and studying new catalyst/support combinations for fuel cell applications. Three publications concern the use of related methods to explore new lithium-sulfur battery concepts.

  7. Synthesis and Gas Phase Thermochemistry of Germanium-Containing Compounds

    Energy Technology Data Exchange (ETDEWEB)

    Classen, Nathan Robert [Iowa State Univ., Ames, IA (United States)

    2002-01-01

    The driving force behind much of the work in this dissertation was to gain further understanding of the unique olefin to carbene isomerization observed in the thermolysis of 1,1-dimethyl-2-methylenesilacyclobutane by finding new examples of it in other silicon and germanium compounds. This lead to the examination of a novel phenylmethylenesilacyclobut-2-ene, which did not undergo olefin to carbene rearrangement. A synthetic route to methylenegermacyclobutanes was developed, but the methylenegermacyclobutane system exhibited kinetic instability, making the study of the system difficult. In any case the germanium system decomposed through a complex mechanism which may not include olefin to carbene isomerization. However, this work lead to the study of the gas phase thermochemistry of a series of dialkylgermylene precursors in order to better understand the mechanism of the thermal decomposition of dialkylgermylenes. The resulting dialkylgermylenes were found to undergo a reversible intramolecular β C-H insertion mechanism.

  8. Synthesis and Gas Phase Thermochemistry of Germanium-Containing Compounds

    Energy Technology Data Exchange (ETDEWEB)

    Nathan Robert Classen

    2002-12-31

    The driving force behind much of the work in this dissertation was to gain further understanding of the unique olefin to carbene isomerization observed in the thermolysis of 1,1-dimethyl-2-methylenesilacyclobutane by finding new examples of it in other silicon and germanium compounds. This lead to the examination of a novel phenylmethylenesilacyclobut-2-ene, which did not undergo olefin to carbene rearrangement. A synthetic route to methylenegermacyclobutanes was developed, but the methylenegermacyclobutane system exhibited kinetic instability, making the study of the system difficult. In any case the germanium system decomposed through a complex mechanism which may not include olefin to carbene isomerization. However, this work lead to the study of the gas phase thermochemistry of a series of dialkylgermylene precursors in order to better understand the mechanism of the thermal decomposition of dialkylgermylenes. The resulting dialkylgermylenes were found to undergo a reversible intramolecular {beta} C-H insertion mechanism.

  9. Diels-Alder Reactions of 6-Hydroxy-2H-pyran-3(6H)-ones with Cyclopentadiene and Its Application for the Synthesis of New Skeletal Oxa-Cage Compounds

    Institute of Scientific and Technical Information of China (English)

    WU Hsien-Jen; LIU HuiChang; CHENG Lui

    2001-01-01

    @@ The 2(5H)-furanone and 3(6H)-pyranone structures are frequently found in natural products, which have a broad range of biological activities. In addition, furanones and pyranones have served as versatile intermediates in the synthesis of a variety of products. 1 Recently, we envisioned that studies on the synthesis and chemistry of heterocyclic cage compounds can greatly expand the scopes and utilities of cage compounds.2 As part of a program that involves the synthesis, chemistry, and applications of heterocyclic cage compounds, we report here the Diels-Alder reactions of 6-hydroxy2H-pyran-3(6H)-ones 1 and 2 with cyclopentadiene and the application of the cycloadducts for the synthesis of oxa-cage compounds 3-6 with new skeleton. Compound 6 is a potential new chiral amino-alcohol.

  10. Synthesis and reactivity of compounds containing ruthenium-carbon, -nitrogen, and -oxygen bonds

    Energy Technology Data Exchange (ETDEWEB)

    Hartwig, J.F.

    1990-12-01

    The products and mechanisms of the thermal reactions of several complexes of the general structure (PMe{sub 3}){sub 4}Ru(X)(Y) and (DMPM){sub 2}Ru(X)(Y) where X and Y are hydride, aryl, and benzyl groups, have been investigated. The mechanism of decomposition depends critically on the structure of the complex and the medium in which the thermolysis is carried out. The alkyl hydride complexes are do not react with alkane solvent, but undergo C-H activation processes with aromatic solvents by several different mechanisms. Thermolysis of (PMe{sub 3}){sub 4}Ru(Ph)(Me) or (PMe{sub 3}){sub 4}Ru(Ph){sub 2} leads to the ruthenium benzyne complex (PMe{sub 3}){sub 4}Ru({eta}{sup 2}-C{sub 6}H{sub 4}) (1) by a mechanism which involves reversible dissociation of phosphine. In many ways its chemistry is analogous to that of early rather than late organo transition metal complexes. The synthesis, structure, variable temperature NMR spectroscopy and reactivity of ruthenium complexes containing aryloxide or arylamide ligands are reported. These complexes undergo cleavage of a P-C bond in coordinated trimethylphosphine, insertion of CO and CO{sub 2} and hydrogenolysis. Mechanistic studies on these reactions are described. The generation of a series of reactive ruthenium complexes of the general formula (PMe{sub 3}){sub 4}Ru(R)(enolate) is reported. Most of these enolates have been shown to bind to the ruthenium center through the oxygen atom. Two of the enolate complexes 8 and 9 exist in equilibrium between the O- and C-bound forms. The reactions of these compounds are reported, including reactions to form oxygen-containing metallacycles. The structure and reactivity of these ruthenium metallacycles is reported, including their thermal chemistry and reactivity toward protic acids, electrophiles, carbon monoxide, hydrogen and trimethylsilane. 243 refs., 10 tabs.

  11. Synthesis of dopamine analogue containing benzeneboronic acid group, a target compound for BNCT

    Energy Technology Data Exchange (ETDEWEB)

    Mizuno, T.; Yoshino, K. [Shinshu Univ., Faculty of Science, Matsumoto, Nagano (Japan); Hiratsuka, J. [Kawasaki Medical School, Dept. of Radiation Oncology, Kurashiki, Okayama (Japan); Ichihashi, M. [Kobe Univ. (Japan). School of Medicine

    2000-10-01

    Melanin synthesis is accentuated in the melanoma cells. DOPA is one of the melanin precursors, and has been found to be the substrates for tyrosinase. Since Dopamine has the similar structure to DOPA, we have thought that the Dopamine containing boron atom has a possibility to be incorporated into the melanin synthesis pathway, resulting in both higher {sup 10}B-delivery and long lasting {sup 10}B-accumulation in melanoma. Thus, we tried to synthesize a new amide compound between Dopamine and p-carboxybenzeneboronic acid (PCBA). (author)

  12. SYNTHESIS ALKANOLAMIDE TETRAHIDROXY OCTADECANOATE COMPOUND FROM CANDLE NUT OIL

    Directory of Open Access Journals (Sweden)

    Daniel Daniel

    2010-06-01

    Full Text Available Candle nut oil could be transesterificated by methanol with concentrated H2SO4 as a catalyst to form fatty acid methyl esther. Methyl linoleate could be separated by Column Chromatography mechanism technic partition from fatty acid methyl ester (FAME mixture, then it was treated by ethanolamine at base condition in benzene as solvent and sodium methylate as a catalyst at reflux condition for 6 hours to form an alkanolamide. Alkanolamide could be epoxydized by tert-buthyl hydroperoxyde and peroxygenase as a catalyst and it was refluxed for 6 hours at 40 °C and nitrogen gas condition to form the epoxy alkanolamide octadecanoate, and then it was hydrolyzed by HCl 0.1 M to form alkanolamide tetrahidroxy octadecanoate (Polyol. Alkanolamide tetrahidroxy octadecanoate could be separated by Column Chromatography using silica gel H 40 and the eluent was the mixture of chloroform, ethyl acetate, formic acid in a ratio 90:10:1 (v/v/v/. Determination of HLB value from alknolamide tetrahydroxy octadecanoate is 13.096. Therefore, this compound was particularly suitable for application as an o/w emulsifiers. All af the reaction steps were confirmed by using FT-IR, 1H-NMR, GC-MS, Gas Chromatography and TLC.   Keywords: Esterification, Candle nut oil, Surfactant, Amidation, Polyol.

  13. Pharmacists Adolf Schall and Ernst Ratzlaff and the synthesis of tabun-like compounds: a brief history.

    Science.gov (United States)

    Petroianu, G A

    2014-10-01

    The history of the synthesis of organophosphate inhibitors of cholinesterase starting with the synthesis of tetraethyl-pyrophosphate by Moschnin(e) and de Clermont and leading to the recognition about half a century later of the toxicity of the phosphor ester by Lange and von Krueger has been told in great detail previously. An almost parallel history -described originally by Bo Holmstedt--exists for organophosphonate inhibitors of cholinesterase starting with the synthesis (1898) in Rostock of diethylamido-ethoxy-phosphoryl-cyanide by the pharmacist Adolph Schall (1870-1957), a graduate student of August Michaelis (1847-1916), the re-examination of the chemical structure of the Schall compound (1903) by Michaelis, recognition (1937) of the toxicity of class by Gerhard Schrader (1903-1990) and confirmation (1951) of the structure by Bo Holmstedt (1919-2002). This short report attempts to shed some light on the life of the pharmacists and chemists involved in the synthesis of the first P-CN organophosphonate inhibitor of cholinesterase, focusing on the two less known pharmacists, the graduate students of Professor Michaelis Adolph Schall and Ernst Ratzlaff (1870-1948).

  14. Proline catalyzed α-aminoxylation reaction in the synthesis of biologically active compounds.

    Science.gov (United States)

    Kumar, Pradeep; Dwivedi, Namrata

    2013-02-19

    The search for new and efficient ways to synthesize optically pure compounds is an active area of research in organic synthesis. Asymmetric catalysis provides a practical, cost-effective, and efficient method to create a variety of complex natural products containing multiple stereocenters. In recent years, chemists have become more interested in using small organic molecules to catalyze organic reactions. As a result, organocatalysis has emerged both as a promising strategy and as an alternative to catalysis with expensive proteins or toxic metals. One of the most successful and widely studied secondary amine-based organocatalysts is proline. This small molecule can catalyze numerous reactions such as the aldol, Mannich, Michael addition, Robinson annulation, Diels-Alder, α-functionalization, α-amination, and α-aminoxylation reactions. Catalytic and enantioselective α-oxygenation of carbonyl compounds is an important reaction to access a variety of useful building blocks for bioactive molecules. Proline catalyzed α-aminoxylation using nitrosobenzene as oxygen source, followed by in situ reduction, gives enantiomerically pure 1,2-diol. This molecule can then undergo a variety of organic reactions. In addition, proline organocatalysis provides access to an assortment of biologically active natural products including mevinoline (a cholesterol lowering drug), tetrahydrolipstatin (an antiobesity drug), R(+)-α-lipoic acid, and bovidic acid. In this Account, we present an iterative organocatalytic approach to synthesize both syn- and anti-1,3-polyols, both enantio- and stereoselectively. This method is primarily based on proline-catalyzed sequential α-aminoxylation and Horner-Wadsworth-Emmons (HWE) olefination of aldehyde to give a γ-hydroxy ester. In addition, we briefly illustrate the broad application of our recently developed strategy for 1,3-polyols, which serve as valuable, enantiopure building blocks for polyketides and other structurally diverse and

  15. Synthesis of Chlorinated Tetracyclic Compounds and Testing for Their Potential Antidepressant Effect in Mice

    Directory of Open Access Journals (Sweden)

    Usama Karama

    2016-01-01

    Full Text Available The synthesis of the tetracyclic compounds 1-(4,5-dichloro-9,10-dihydro-9,10-ethanoanthracen-11-yl-N-methylmethanamine (5 and 1-(1,8-dichloro-9,10-dihydro-9,10-ethanoanthracen-11-yl-N-methylmethanamine (6 as a homologue of the anxiolytic and antidepressant drugs benzoctamine and maprotiline were described. The key intermediate aldehydes (3 and (4 were successfully synthesized via a [4 + 2] cycloaddition between acrolein and 1,8-dichloroanthracene. The synthesized compounds were investigated for antidepressant activity using the forced swimming test. Compounds (5, (6 and (3 showed significant reduction in the mice immobility indicating significant antidepressant effects. These compounds significantly reduced the immobility times at a dose 80 mg/kg by 84.0%, 86.7% and 71.1% respectively.

  16. Design, synthesis and biological evaluation of novel aminothiazoles as antiviral compounds acting against human rhinovirus.

    Science.gov (United States)

    Décor, Anne; Grand-Maître, Chantal; Hucke, Oliver; O'Meara, Jeff; Kuhn, Cyrille; Constantineau-Forget, Léa; Brochu, Christian; Malenfant, Eric; Bertrand-Laperle, Mégan; Bordeleau, Josée; Ghiro, Elise; Pesant, Marc; Fazal, Gulrez; Gorys, Vida; Little, Michael; Boucher, Colette; Bordeleau, Sylvain; Turcotte, Pascal; Guo, Tim; Garneau, Michel; Spickler, Catherine; Gauthier, Annick

    2013-07-01

    We describe here the design, synthesis and biological evaluation of antiviral compounds acting against human rhinovirus (HRV). A series of aminothiazoles demonstrated pan-activity against the HRV genotypes screened and productive structure-activity relationships. A comprehensive investigational library was designed and performed allowing the identification of potent compounds with lower molecular weight and improved ADME profile. 31d-1, 31d-2, 31f showed good exposures in CD-1 mice. The mechanism of action was discovered to be a host target: the lipid kinase phosphatidylinositol 4-kinase III beta (PI4KIIIß). The identification of the pan-HRV active compound 31f combined with a structurally distinct literature compound T-00127-HEV1 allowed the assessment of target related tolerability of inhibiting this kinase for a short period of time in order to prevent HRV replication.

  17. Cu(II AND Zn(II COMPLEX COMPOUNDS WITH BIGUANIDES AROMATIC DERIVATIVES. SYNTHESIS, CHARACTERIZATION, BIOLOGICAL ACTIVITY

    Directory of Open Access Journals (Sweden)

    Ticuţa Negreanu-Pîrjol

    2011-05-01

    Full Text Available In this paper we report the synthesis, physical-chemical characterization and antimicrobial activity of some new complex compounds of hetero-aromatic biguanides ligands, chlorhexidine base (CHX and chlorhexidine diacetate (CHXac2 with metallic ions Cu(II and Zn(II, in different molar ratio. The synthesized complexes were characterized by elemental chemical analysis and differential thermal analysis. The stereochemistry of the metallic ions was determined by infrared spectra, UV-Vis, EPR spectroscopy and magnetic susceptibility in the aim to establish the complexes structures. The biological activity of the new complex compounds was identified in solid technique by measuring minimum inhibition diameter of bacterial and fungal culture, against three standard pathogen strains, Escherichia coli ATCC 25922, Staphilococcus aureus ATCC 25923 and Candida albicans ATCC 10231. The results show an increased specific antimicrobial activity for the complexes chlorhexidine:Cu(II 1:1 and 1:2 compared with the one of the Zn(II complexes.

  18. Synthesis of Melamine-d6 and the Feasibility of Deuterium Labeled Compounds as Internal Standard

    Directory of Open Access Journals (Sweden)

    GUO Yang-zhen

    2015-11-01

    Full Text Available S-triazine is an important chemical intermediate. Melamine belongs to s-triazine, which has been widely used as an additive in the food industry. To study the stable isotope labeling method of heterocyclic triazine compounds and its application, one step synthesis of melamine-d6 was achieved with a yield of 30% (calculate in ND4OD, which started from ND4OD by the reaction with cyanuric chloride. According to the exchange mechanism of H/D, the feasibility and the necessary conditions were discussed for applying deuterium labeled compounds in isotope dilution mass spectrometry method.

  19. Metabolic Diversity for Degradation, Detection, and Synthesis of Nitro Compounds and Toxins

    Science.gov (United States)

    2012-07-08

    S. F., and J. C. Spain. 2012. Growth of marine bacteria on the natural organophosphate (S)-cinnamoylphosphoramide. abstr. Q-1497, Annual Meeting...awareness of the widespread synthesis of nitro organic compounds of natural origin in a variety of marine and terrestrial ecosystems (Fig. 1, (37, 52...formed in bacteria by both nitric oxide synthease (NOS) (1) and by nitrite reductase (10). In soil bacteria, particularly actinomycetes , NOS catalyzes

  20. Design, synthesis and in vitro evaluation of novel anti-cancer compounds

    OpenAIRE

    McCormack, Emmet Martin

    2003-01-01

    The purpose of this thesis was the design, synthesis and in vitro appraisal of a novel class of ITP/APN dual inhibitory compounds. Additionally, a class of novel biaryls, which were synthesised within the research group, were assayed to evaluate their ability to inhibit tubulin polymerisation (ITP). The introductory chapter commences with brief overview of the history of cancer and role of natural products in conventional chemotherapeutic regimes and adjuvant immunotherapies. Subsequently, th...

  1. Compostos alfa-diazo carbonílicos: uma estratégia atraente para a síntese orgânica alpha-diazo carbonyl compounds: an atractive estrategy in organic synthesis

    Directory of Open Access Journals (Sweden)

    Vítor F. Ferreira

    2001-08-01

    Full Text Available Diazocarbonyl compounds are a very important class of organic substances which have a long history of useful aplications in organic chemistry. The focus of this report deals with the use of diazocarbonyl compounds in a ariety of important reactions and their application in organic synthesis. These reactions are briefly summarized showing their broad scope.

  2. Synthesis of 2-methoxy-6-oxo-1, 4, 2-diazaphosphorinane-2-oxide, A New Potential Antitumor Phosphorus Heterocycle Compound

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    2-methoxy-6-oxo-1, 4, 2-diazaphosphorinane-2-oxide 8, phosphorus counterpart of 2, 6-dioxopiperazine, was synthesized as antitumor agent. The new phosphorus heterocycle compound 8 is the key intermediate in the synthesis of phosphorus counterpart of bisdioxopiperazine.

  3. Synthesis of two-dimensional TlxBi1−x compounds and Archimedean encoding of their atomic structure

    Science.gov (United States)

    Gruznev, Dimitry V.; Bondarenko, Leonid V.; Matetskiy, Andrey V.; Mihalyuk, Alexey N.; Tupchaya, Alexandra Y.; Utas, Oleg A.; Eremeev, Sergey V.; Hsing, Cheng-Rong; Chou, Jyh-Pin; Wei, Ching-Ming; Zotov, Andrey V.; Saranin, Alexander A.

    2016-01-01

    Crystalline atomic layers on solid surfaces are composed of a single building block, unit cell, that is copied and stacked together to form the entire two-dimensional crystal structure. However, it appears that this is not an unique possibility. We report here on synthesis and characterization of the one-atomic-layer-thick TlxBi1−x compounds which display quite a different arrangement. It represents a quasi-periodic tiling structures that are built by a set of tiling elements as building blocks. Though the layer is lacking strict periodicity, it shows up as an ideally-packed tiling of basic elements without any skips or halting. The two-dimensional TlxBi1−x compounds were formed by depositing Bi onto the Tl-covered Si(111) surface where Bi atoms substitute appropriate amount of Tl atoms. Atomic structure of each tiling element as well as arrangement of TlxBi1−x compounds were established in a detail. Electronic properties and spin texture of the selected compounds having periodic structures were characterized. The shown example demonstrates possibility for the formation of the exotic low-dimensional materials via unusual growth mechanisms. PMID:26781340

  4. Synthesis of two-dimensional TlxBi1-x compounds and Archimedean encoding of their atomic structure

    Science.gov (United States)

    Gruznev, Dimitry V.; Bondarenko, Leonid V.; Matetskiy, Andrey V.; Mihalyuk, Alexey N.; Tupchaya, Alexandra Y.; Utas, Oleg A.; Eremeev, Sergey V.; Hsing, Cheng-Rong; Chou, Jyh-Pin; Wei, Ching-Ming; Zotov, Andrey V.; Saranin, Alexander A.

    2016-01-01

    Crystalline atomic layers on solid surfaces are composed of a single building block, unit cell, that is copied and stacked together to form the entire two-dimensional crystal structure. However, it appears that this is not an unique possibility. We report here on synthesis and characterization of the one-atomic-layer-thick TlxBi1-x compounds which display quite a different arrangement. It represents a quasi-periodic tiling structures that are built by a set of tiling elements as building blocks. Though the layer is lacking strict periodicity, it shows up as an ideally-packed tiling of basic elements without any skips or halting. The two-dimensional TlxBi1-x compounds were formed by depositing Bi onto the Tl-covered Si(111) surface where Bi atoms substitute appropriate amount of Tl atoms. Atomic structure of each tiling element as well as arrangement of TlxBi1-x compounds were established in a detail. Electronic properties and spin texture of the selected compounds having periodic structures were characterized. The shown example demonstrates possibility for the formation of the exotic low-dimensional materials via unusual growth mechanisms.

  5. Synthesis of two-dimensional Tl(x)Bi(1-x) compounds and Archimedean encoding of their atomic structure.

    Science.gov (United States)

    Gruznev, Dimitry V; Bondarenko, Leonid V; Matetskiy, Andrey V; Mihalyuk, Alexey N; Tupchaya, Alexandra Y; Utas, Oleg A; Eremeev, Sergey V; Hsing, Cheng-Rong; Chou, Jyh-Pin; Wei, Ching-Ming; Zotov, Andrey V; Saranin, Alexander A

    2016-01-19

    Crystalline atomic layers on solid surfaces are composed of a single building block, unit cell, that is copied and stacked together to form the entire two-dimensional crystal structure. However, it appears that this is not an unique possibility. We report here on synthesis and characterization of the one-atomic-layer-thick Tl(x)Bi(1-x) compounds which display quite a different arrangement. It represents a quasi-periodic tiling structures that are built by a set of tiling elements as building blocks. Though the layer is lacking strict periodicity, it shows up as an ideally-packed tiling of basic elements without any skips or halting. The two-dimensional Tl(x)Bi(1-x) compounds were formed by depositing Bi onto the Tl-covered Si(111) surface where Bi atoms substitute appropriate amount of Tl atoms. Atomic structure of each tiling element as well as arrangement of Tl(x)Bi(1-x) compounds were established in a detail. Electronic properties and spin texture of the selected compounds having periodic structures were characterized. The shown example demonstrates possibility for the formation of the exotic low-dimensional materials via unusual growth mechanisms.

  6. Hybrid Compounds Strategy in the Synthesis of Oleanolic Acid Skeleton-NSAID Derivatives

    Directory of Open Access Journals (Sweden)

    Anna Pawełczyk

    2016-04-01

    Full Text Available The current study focuses on the synthesis of several hybrid individuals combining a natural oleanolic acid skeleton and synthetic nonsteroidal anti-inflammatory drug moieties (NSAIDs. It studied structural modifications of the oleanolic acid structure by use of the direct reactivity of hydroxyl or hydroxyimino groups at position C-3 of the triterpenoid skeleton with the carboxylic function of anti-inflammatory drugs leading to new perspective compounds with high potential pharmacological activities. Novel ester- and iminoester-type derivatives of oleanolic unit with the different NSAIDs, such as ibuprofen, aspirin, naproxen, and ketoprofen, were obtained and characterized. Moreover, preliminary research of compounds obtaining structure stability under acidic conditions was examined and the PASS method of prediction of activity spectra for substances was used to estimate the potential biological activity of these compounds.

  7. Synthesis and biological activity of sulfur compounds showing structural analogy with combretastatin A-4

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Edson dos A. dos; Prado, Paulo C.; Carvalho, Wanderley R. de; Lima, Ricardo V. de; Beatriz, Adilson; Lima, Denis P. de, E-mail: denis.lima@ufms.br [Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande, MS (Brazil). Departamento de Quimica; Hamel, Ernest [Screening Technologies Branch, Developmental Therapeutics Program, Division of Cancer Treatment and Diagnosis, National Cancer Institute at Frederick, National Institutes of Health, Frederick, MD (United States); Dyba, Marzena A. [Basic Science Program , SAIC-Frederick, Inc., Structural Biophysics Laboratory National Cancer Institute, Frederick, MD (United States); Albuquerque, Sergio [Universidade de Sao Paulo (USP), Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas

    2013-09-01

    We extended our previous exploration of sulfur bridges as bioisosteric replacements for atoms forming the bridge between the aromatic rings of combretastatin A-4. Employing coupling reactions between 5-iodo-1,2,3-trimethoxybenzene and substituted thiols, followed by oxidation to sulfones with m-CPBA, different locations for attaching the sulfur atom to ring A through the synthesis of nine compounds were examined. Antitubulin activity was performed with electrophoretically homogenous bovine brain tubulin, and activity occurred with the 1,2,3-trimethoxy-4-[(4-methoxyphenyl)thio]benzene (12), while the other compounds were inactive. The compounds were also tested for leishmanicidal activity using promastigote forms of Leishmania braziliensis (MHOM/BR175/M2904),and the greatest activity was observed with 1,2,3-trimethoxy-4-(phenylthio)benzene (10) and 1,2,3-trimethoxy-4-[(4-methoxyphenyl) sulfinyl]benzene (15). (author)

  8. Mesoporous Silica Based Gold Catalysts: Novel Synthesis and Application in Catalytic Oxidation of CO and Volatile Organic Compounds (VOCs

    Directory of Open Access Journals (Sweden)

    Leonarda F. Liotta

    2013-10-01

    Full Text Available Gold nanoparticles, particularly with the particle size of 2–5 nm, have attracted increasing research attention during the past decades due to their surprisingly high activity in CO and volatile organic compounds (VOCs oxidation at low temperatures. In particular, CO oxidation below room temperature has been extensively studied on gold nanoparticles supported on several oxides (TiO2, Fe2O3, CeO2, etc.. Recently, mesoporous silica materials (such as SBA-15, MCM-41, MCM-48 and HMS possessing ordered channel structures and suitable pore diameters, large internal surface areas, thermal stabilities and excellent mechanical properties, have been investigated as suitable hosts for gold nanoparticles. In this review we highlight the development of novel mesoporous silica based gold catalysts based on examples, mostly from recently reported results. Several synthesis methods are described herein. In detail we report: the modification of silica with organic functional groups; the one-pot synthesis with the incorporation of both gold and coupling agent containing functionality for the synthesis of mesoporous silica; the use of cationic gold complexes; the synthesis of silica in the presence of gold colloids or the dispersion of gold colloids protected by ligands or polymers onto silica; the modification of silica by other metal oxides; other conventional preparation methods to form mesoporous silica based gold catalysts. The gold based catalysts prepared as such demonstrate good potential for use in oxidation of CO and VOCs at low temperatures. From the wide family of VOCs, the oxidation of methanol and dimethyldisulfide has been addressed in the present review.

  9. Design, Synthesis, and Structural Analysis of Divalent N(I) Compounds and Identification of a New Electron-Donating Ligand.

    Science.gov (United States)

    Bharatam, Prasad V; Arfeen, Minhajul; Patel, Neha; Jain, Priyanka; Bhatia, Sonam; Chakraborti, Asit K; Khullar, Sadhika; Gupta, Vijay; Mandal, Sanjay K

    2016-01-18

    The dative-bond representation (L→E) in compounds with main group elements (E) has triggered extensive debate in the recent past. The scope and limits of this nonclassical coordination bond warrant comprehensive exploration. Particularly compounds with (L→N←L')(+) arrangement are of special interest because of their therapeutic importance. This work reports the design and synthesis of novel chemical species with the general structural formula (L→N←L')(+) carrying the unusual ligand cyclohexa-2,5-diene-4-(diaminomethynyl)-1-ylidene. Four species belonging to the (L→N←L')(+) class carrying this unconventional ligand were synthesized. Quantum chemical and X-ray diffraction analyses showed that the electronic and geometric parameters are consistent with those of already reported divalent N(I) compounds. The molecular orbital analysis, geometric parameters, and spectral data clearly support the L→N and N←L' interactions in these species. The newly identified ligand has the properties of a reactive carbene and high nucleophilicity.

  10. Synthesis and solid state structures of Chalcogenide compounds of Imidazolin-2-ylidene-1,1-Diphenyl-phosphinamine

    Indian Academy of Sciences (India)

    Naktode Kishor; Suman Das; Abhinanda Kundu; Hari Pada Nayek; Tarun K Panda

    2016-03-01

    We report the synthesis and solid state structures of 1,3-di-aryl-imidazolin-2-ylidine-1,1-diphenylphosphinamine [(aryl=mesityl (1a) and aryl=2,6-diisopripyl (1b)] and their chalcogenide compounds 3-di-aryl-imidazolin-2-ylidine-P, P-diphenylphosphinicamide (2a,b), 1,3-di-aryl-imidazolin-2-ylidine-P,P diphenyl-phosphinothioicamide (3a,b) and 1,3-diaryl-imidazolin-2-ylidine-P,P -diphenyl-phosphinoselenoicamide (4a,b).The compounds 1a,b were prepared in good yield by the reaction of 1,3-di-aryl-imidazolin-2-imine and chlorodiphenylphosphine in the presence of triethylamine in toluene. The reactions of 1a,b with elemental sulphur and selenium afforded the corresponding chalcogenide compounds 3a,b and 4a,b respectively.The corresponding oxo- derivative (2a,b) was obtained by reacting compound 1a,b with 30% aqueous hydrogen peroxide in THF. The molecular structures of 1a, 2a, 3a and 4a,b have been established by single crystal X-ray diffraction analyses. The molecular structures reveal that even C1–N1–P1 angle (124.62o) in compound 1a is less obtuse compared to the corresponding C1–N1–Si1 angles (157.8o) observed in related N-silylated 2-iminoimidazolines and trimethylsilyl iminophosphoranes. C1–N1–P1 angles are further widened in compounds 2a, 3a, and 4a,b due to the attachment of chalcogen atoms onto phosphorus atom.

  11. Synthesis and evaluation of octocrylene-inspired compounds for UV-filter activity

    Directory of Open Access Journals (Sweden)

    Hudson C. Polonini

    2014-07-01

    Full Text Available Octocrylene (2-ethylhexyl 2-cyano-3,3-diphenyl-2-propenoate is present in several sunscreens and is known to work synergistically with UV filters. We prepared eight octocrylene-related compounds to test their photoprotective activities by measuring diffuse transmittance. The compounds had varied photoprotection profiles, with Sun Protection Factors (SPF ranging from 1 to 5 and UVA Protection Factors (UVAPF ranging from 1 to 8. Compounds 4, 5, and 7 showed the best protection against UVB sunrays, while compounds 5, 6, and 7 presented the best results for protection from UVA, so compound 7 had the most balanced protection overall. Results for compounds 4, 8, and 9 are reported for the first time in the literature.

  12. Synthesis, investigation and practical application in lithium batteries of some compounds based on vanadium oxides

    Science.gov (United States)

    Shembel, E.; Apostolova, R.; Nagirny, V.; Aurbach, D.; Markovsky, B.

    In this paper, we investigate the inter-relationship between the conditions of the electrochemical synthesis of vanadium oxide compounds, their structural and morphological characteristics, kinetic parameters of the redox processes, and charge-discharge performance of lithium batteries with vanadium oxide cathodes. The materials studied were V 2O 5- y oxides and those with inserted sodium ions (Na-vanadium oxide compounds, Na-VOC) obtained electrochemically in the form of compact deposits on a metal substrate. The electrochemical synthesis of the oxides has been performed from aqueous vanadyl sulphate solutions. Optimal synthesis conditions (current density, pH, temperature, vanadyl sulphate and sodium sulphate concentrations), and subsequent optimal thermal treatment of the oxides, which provide high electrochemical activity of the cathode material and good adhesion of the oxide to the metal substrate, have been elucidated. A correlation between the structure of the vanadium oxides and Na-VOC, their morphology, impedance characteristics of the cathode, and lithium-ion solid state diffusion in the host cathode bulk has been established and discussed. A combination of analytical techniques (XRD, IR spectroscopy, TGA, BET, SEM) and electrochemical methods (cyclic voltammetry, chronopotentiometry, GITT, EIS) has been used in this study.

  13. Ultrafast Synthesis and Related Phase Evolution of Mg2Si and Mg2Sn Compounds

    Science.gov (United States)

    Zhang, Qiang; Lu, Qiangbing; Yan, Yonggao; Su, Xianli; Tang, Xinfeng

    2017-02-01

    Both Mg2Si and Mg2Sn compounds were synthesized by an ultra-fast self-propagating high-temperature synthesis (SHS) method. The data regarding SHS were obtained via theoretical calculation combined with experiments, showing that the adiabatic temperature T ad and ignition temperature T ig of Mg2Si are a little higher than those of Mg2Sn. The mechanism of phase evolution and the concomitant microstructure evolution during the synthesis process of Mg2Si and Mg2Sn compounds were investigated by adopting SHS technique coupled with a sudden quenching treatment. Differential scanning calorimetry (DSC), field emission scanning electron microscopy (FESEM), and x-ray powder diffraction (XRD) results indicate that Mg2Si compound can be directly synthesized through the reaction of Mg and Si elements at around 850 K. Correspondingly, the formation of Mg2Sn needs to undergo melting of Sn and the subsequent feeble reaction between Mg and Sn elements before the large scale transformation at 730 K. As the groundwork, this research embodies great significance for future study on the ultrafast SHS process of the ternary Mg2Si1-x Sn x solid solutions.

  14. Synthesis of compounds related to the anti-migraine drug eletriptan hydrobromide

    Directory of Open Access Journals (Sweden)

    Suri Babu Madasu

    2012-08-01

    Full Text Available Eletriptan hydrobromide (1 is a selective serotonin (5-HT1 agonist, used for the acute treatment of the headache phase of migraine attacks. During the manufacture of eletriptan hydrobromide the formation of various impurities were observed and identified by LC–MS. To control the formation of these impurities during the preparation of active pharmaceutical ingredients, the structure of the impurities must be known. Major impurities of the eletriptan hydrobromide synthesis were prepared and characterized by using various spectroscopic techniques, i.e., mass spectroscopy, FTIR , 1H NMR, 13C NMR/DEPT, and further confirmed by co-injection in HPLC. The present study will be of great help in the synthesis of highly pure eletriptan hydrobromide related compounds.

  15. Design and Synthesis of Polypyrazolyl Compounds as a New Type of Versatile Building Blocks

    Institute of Scientific and Technical Information of China (English)

    LI,Sheng-Hui; HUANG,Hai-Ping; YU,Shu-Yan; LI,Xian-Ping

    2006-01-01

    The design and synthesis of novel polypyrazolyl aromatic bridging ligands 1,3,5-tris(3,5-dimethyl-1H-pyrazol-4-yl)benzene and 2,4,6-tris(4-(3,5-dimethyl-1H-pyrazol-4-yl)phenyl)-1,3,5-triazine from simple starting materials mesitylene and p-tolunitrile were reported.

  16. Phenolic compounds in cultures of tissues of tea plants and the effect of light on their synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Koretskaya, T.F.; Zaprometov, M.N.

    1975-01-01

    Stem and leaf calluses of tea plants (Camellia sinensis) retain the capacity for synthesis of phenolic compounds. The content of phenolic compounds comprises 2 to 5 percent of dry weight, the main share (80 to 95 percent) belonging to catechins and leucoanthocyans, including their polymeric forms. The following compounds were detected in callus tissue: (--)-epicatechin, (+)-catechin, two leucoanthocyans, and several unidentified phenolic compounds that fluoresce in UV. (--)-Epicatechin is predominant. In contrast to tissues of an intact plant, the callus does not contain gallocatechins or free gallic acid under the given cultivation conditions. The content of phenolic compounds changes in proportion to callus growth, their greatest amount being formed during the phase of intensive growth. Light stimulates synthesis of phenolic compounds, including the most reduced group of flavonoids, viz., leucoanthocyans and catechins.

  17. Synthesis of reported and revised structures of amathamide D and synthesis of convolutamine F, H and lutamide A, C.

    Science.gov (United States)

    Khan, Faiz Ahmed; Ahmad, Saeed

    2012-03-01

    Total synthesis of the published structure of amathamide D is described. Methyl 2,3,4-tribromo-5-hydroxybenzoate was selected as starting compound because it is readily accessible via acid-mediated Grob fragmentation-aromatization reaction of 1,4,5,6-tetrabromo-7,7-dimethoxybicyclo[2.2.1]hept-5-en-2-one. The aforementioned ester was transformed into the reported structure of amathamide D through methylation of a hydroxyl group and conversion of the ester moiety to a β-aminoethyl side chain. The NMR data of the synthetic compound did not conform to the reported natural product structure possessing contiguously positioned β-aminoethyl side chain, a set of three adjacent bromines, and a methyl ether linkage on the phenyl ring. This prompted us to redefine the natural product structure by synthesizing a product whose spectral data exactly matched with the reported data of amathamide D. The convolutamine H, with completely substituted phenyl ring adorned with an extra methyl ether functional group, has also been synthesized by application of Grob fragmentation-aromatization strategy to 3-(benzyloxy)-1,4,5,6-tetrabromo-7,7-dimethoxybicyclo[2.2.1]hept-5-en-2-one. This approach furnished directly methyl 2,3,4-tribromo-5,6-dimethoxybenzoate, which was converted straightforwardly into convolutamine H. Further, synthesis of convolutamine F and lutamide A and C is also described.

  18. Synthesis of an opine-like compound, a rhizopine, in alfalfa nodules is symbiotically regulated.

    OpenAIRE

    Murphy, P J; Heycke, N; Trenz, S P; Ratet, P.; de Bruijn, F J; Schell, J.

    1988-01-01

    We show that the promoter of the mos locus, which encodes genes required for the synthesis of a nodule-specific, opine-like compound, a rhizopine, in alfalfa nodules is regulated by the symbiotic nitrogen-fixation regulatory gene nifA. The 5'-regulatory region and amino-terminal end of the first open reading frame of the mos locus are highly homologous to the 5'-regulatory region and amino-terminal portion of the Rhizobium meliloti nifH gene. The coordinate regulation of mos and nif genes sug...

  19. Synthesis of (iso)quinoline, (iso)coumarin and (iso)chromene derivatives from acetylene compounds

    Science.gov (United States)

    Ryabukhin, D. S.; Vasilyev, A. V.

    2016-06-01

    Published data on the methods of synthesis of quinoline, isoquinoline, coumarin, isocoumarin, chromene and isochromene derivatives from acetylene compounds are summarized. The reactions catalyzed by metal complexes (Pd, Pt, Ru, Rh, Au, Ag, Ni, Cu, etc.) and transformations induced by various electrophilic reagents (Brynsted and Lewis acids) are considered. Moieties of the mentioned heterocyclic systems are present in many biologically active natural products and pharmaceutical agents. Besides, derivatives of these heterocycles are used in the manufacture of catalysts, dyes, perfumery and cosmetic products, corrosion inhibitors and so on. The bibliography includes 211 references.

  20. Synthesis of superheavy elements and dinuclear-system concept of compound-nucleus formation

    Energy Technology Data Exchange (ETDEWEB)

    Antonenko, N.V.; Adamian, G.G.; Cherepanov, E.A. [Joint Institute for Nuclear Research, Dubna (Russian Federation)] [and others

    1996-12-31

    Dinuclear system concept is applied to the analysis of reactions used for the synthesis of elements with Z = 110, 112, 114, and 116. The inner fusion barriers obtained for these reactions are in good agreement with the experimental estimations resulted from the excitation energies of compound nuclei. A model is suggested for the calculation of the competition between complete fusion and quasifission in reactions with heavy nuclei. The fusion rate through the inner fusion barrier in mass asymmetry is found by using the multidimensional Kramers-type stationary solution of the Fokker-Planck equation. The influence of dissipative effects on the dynamics of nuclear fusion is considered.

  1. Overcoming Chloroquine Resistance in Malaria: Design, Synthesis, and Structure-Activity Relationships of Novel Hybrid Compounds.

    Science.gov (United States)

    Boudhar, Aicha; Ng, Xiao Wei; Loh, Chiew Yee; Chia, Wan Ni; Tan, Zhi Ming; Nosten, Francois; Dymock, Brian W; Tan, Kevin S W

    2016-05-01

    Resistance to antimalarial therapies, including artemisinin, has emerged as a significant challenge. Reversal of acquired resistance can be achieved using agents that resensitize resistant parasites to a previously efficacious therapy. Building on our initial work describing novel chemoreversal agents (CRAs) that resensitize resistant parasites to chloroquine (CQ), we herein report new hybrid single agents as an innovative strategy in the battle against resistant malaria. Synthetically linking a CRA scaffold to chloroquine produces hybrid compounds with restored potency toward a range of resistant malaria parasites. A preferred compound, compound 35, showed broad activity and good potency against seven strains resistant to chloroquine and artemisinin. Assessment of aqueous solubility, membrane permeability, and in vitro toxicity in a hepatocyte line and a cardiomyocyte line indicates that compound 35 has a good therapeutic window and favorable drug-like properties. This study provides initial support for CQ-CRA hybrid compounds as a potential treatment for resistant malaria.

  2. Synthesis and biological screening by novel hybrid fluorocarbon hydrocarbon compounds for use as artificial blood substitutes

    Science.gov (United States)

    Moacanin, J.; Scherer, K.; Toronto, A.; Lawson, D.; Terranova, T.; Yavrouian, A.; Astle, L.; Harvey, S.; Kaaelble, D. H.

    1979-01-01

    A series of hybrid fluorochemicals of general structure R(1)R(2)R(3)CR(4) was prepared where the R(i)'s (i=1,2,3) is a saturated fluoroalkyl group of formula C sub N F sub 2n+1, and R(4) is an alkyl group C sub n H sub 2n+1 or a related moiety containing amino, ether, or ester functions but no CF bonds. Compounds of this class containing approximately eight to twenty carbons total have physical properties suitable for use as the oxygen carrying phase of fluorochemical emulsion artificial blood. The chemical synthesis, and physical and biological testing of pure single isomers of the proposed artificial blood candidate compounds are included. Significant results are given.

  3. [Emission characteristics and hazard assessment analysis of volatile organic compounds from chemical synthesis pharmaceutical industry].

    Science.gov (United States)

    Li, Yan; Wang, Zhe-Ming; Song, Shuang; Xu, Zhi-Rong; Xu, Ming-Zhu; Xu, Wei-Li

    2014-10-01

    In this study, volatile organic compounds (VOCs) released from chemical synthesis pharmaceutical industry in Taizhou, Zhejiang province were analyzed quantitatively and qualitatively. The total volatile organic compounds (TVOCs) was in the range of 14.9-308.6 mg · m(-3). Evaluation models of ozone formation potentials (OFP) and health risk assessment were adopted to preliminarily assess the environmental impact and health risk of VOCs. The results showed that the values of OFP of VOCs were in the range of 3.1-315.1 mg · m(-3), based on the maximum incremental reactivity, the main principal contribution was toluene, tetrahydrofuran (THF), acetic ether etc. The non-carcinogenic risk and the carcinogen risk fell in the ranges of 9.48 x 10(-7)-4.98 x 10(-4) a(-1) and 3.17 x 10(-5)- 6.33 x 10(-3). The principal contribution of VOCs was benzene, formaldehyde and methylene chloride.

  4. Easy Access to a Cyclic Key Intermediate for the Synthesis of Trisporic Acids and Related Compounds

    Directory of Open Access Journals (Sweden)

    José A. González-Delgado

    2014-02-01

    Full Text Available The synthesis of a cyclohexane skeleton possessing different oxygenated functional groups at C–3, C–8 and C–9, and a D1,6-double bond has been accomplished in 10 steps with an overall 17% yield. This compound is a key intermediate for access to a wide range of compounds of the bioactive trisporoid family. The synthetic sequence consists of the preparation of a properly functionalized epoxygeraniol derivative, and its subsequent stereoselective cyclization mediated by Ti(III. This last step implies a domino process that starts with a homolytic epoxide opening followed by a radical cyclization and regioselective elimination. This concerted process gives access to the cyclohexane moiety with stereochemical control of five of its six carbon atoms.

  5. Synthesis, structure, and properties of a novel family of layered transition nitride compounds

    Science.gov (United States)

    Weil, Kenneth Scott

    The chemical properties of nitrogen present a number of difficulties in the synthesis of nitride compounds. Most of these compounds have small free energies of formation due in part to the strong triple bond of N2. Thus the standard solid state approach of synthesizing compounds from a mixture of their constituents at high reaction temperatures is generally precluded. A general alternative to solid state synthesis is the molecularly mixed precursor route. The primary advantage of this approach is the control of composition. This concept has been demonstrated in this study through the use of a nonaqueous, complexed co-precipitation technique to synthesize a number of new ternary nitride compounds, including the a new nitride phase, CrWN2, and four series of substitutional variations of this compound, as wen as twelve additional new compounds crystallizing in the layered dinitride, eta-nitride, and pi-nitride crystal structures. The layered nitride, CrWN2, is the focal point of this thesis. The details of its crystal and defect structure, synthesis, properties, and substitutional chemistry have been examined and discussed within. Briefly, this compound crystallizes in a trigonal structure and consists of alternating layers of chromium in octahedral coordination with nitrogen and tungsten in trigonal prismatic coordination with nitrogen. Microstructurally, the nitride frequently displays twinning and the formation of coherent rock salt structured intergrowth defects. As mentioned above, the layered nitride evolves from a co-precipitated precursor; a fine mixture of [Cr(NH3)6]Cl 2 and WOCl2·3NH3. Upon heat treatment in an ammonia atmosphere, the two transition metal complexes separately decompose into their non-complexed chloride state, i.e. CrCl2 and WOCl 2, before reacting with each other and the ambient ammonia atmosphere between 420°C and 570°C to form a glassy oxynitrochloride phase, CrWO 1.01N0.36Cl2.45. Around 600°C, this compound undergoes ammonolysis

  6. Synthesis of some derivatives of compounds β-aminoketonic through Mannich reaction by usingbiocatalysts

    Directory of Open Access Journals (Sweden)

    Ana Claudia S. Lima

    2012-06-01

    Full Text Available The Mannich reaction is one of the most widely used reactions in organic chemistry, and also one of the first examples of a multicomponent reaction already described on the literature. This reaction results in β-aminocarbonylated compounds which allow the generation of several structures that can be used in the synthesis of both biologically active molecules, and natural products, however, just a few synthetic routes resulting in the formation of β-aminocarbonylated compound are known. In this sense, new methodologies have been developed by involving new catalysts or chiral auxiliaries in the synthesis of β-aminocarbonylated compounds with biological activity. One of these methodologies is the biocatalysis, which is a technique that uses biological catalysts, like enzymes or micro-organisms to convert a substrate in a limited number of enzymatic steps. The use of micro-organisms, plants or isolated enzymes as chiral catalysts has proportioned a significant advance in the synthetic chemistry, because it is known that the biocatalysts have selective catalytic sites that afford the formation of enantiomerically pure products and which is extremely important, because it is known that differences of the chirality may have tragic or spectacular effects in humans. Concerning to the environmental issue, the biocatalysis is placed within the context of a new philosophy called Green Chemistry. However, in the State of Mato Grosso do Sul the researches involving this issue of biocatalysis are still incipient once that by the year of 2010 there was only one research group focused on this themeregistered in the Lattes Platform in the State. Because of the need of support to the researches focused on this issue in the State of Mato Grosso do Sul and to evaluate thebiocatalytic potential of different lineage of microorganisms and enzymes in the synthesis of compounds β-aminoketonic through Mannich reaction it was proposed the use of someenzymes such as

  7. Synthesis of adenine, guanine, cytosine, and other nitrogen organic compounds by a Fischer-Tropsch-like process.

    Science.gov (United States)

    Yang, C. C.; Oro, J.

    1971-01-01

    Study of the formation of purines, pyrimidines, and other bases from CO, H2, and NH3 under conditions similar to those used in the Fischer-Tropsch process. It is found that industrial nickel/iron alloy catalyzes the synthesis of adenine, guanine, cytosine, and other nitrogenous compounds from mixtures of CO, H2, and NH3 at temperatures of about 600 C. Sufficient sample was accumulated to isolate as solid products adenine, guanine, and cytosine, which were identified by infrared spectrophotometry. In the absence of nickel/iron catalyst, at 650 C, or in the presence of this catalyst, at 450 C, no purines or pyrimidines were synthesized. These results confirm and extend some of the work reported by Kayatsu et al. (1968).

  8. Synthesis and properties of a new superconducting compound (ZrCuxSe2)

    Science.gov (United States)

    Generoso, Ana Carolina; Baptista, Naiara; Renosto, Sergio; Jefferson Machado, Antonio

    2012-02-01

    Since the discovery of superconductivity in chalcogenides in Fe-Se system and in iron pnictides much attention have been give for synthesis of new materials which can exhibit superconductivity. Within this context in this work we show results which suggest the existence of a new selenite intercalate with copper atoms in the ZrCuxSe2 nominal composition, where x is 0.1 <= x <= 0.4 interval. A superconductor behavior begins in the ZrCu0.3Se2 with superconducting critical temperature close to 9.0 K. ZrSe2 is a compound which crystallize in the hexagonal symmetry with CdI2 prototype structure belongs to the space group P-32/m1. Indeed, copper is intercalating between Se-Se which have van der Walls interaction in the ZrSe2 compound. This intercalation with copper atoms, produce superconductivity in the matrix compound (ZrSe2) which is not superconductor. The copper intercalation in the matrix compound crystallizes in a LiCrS2 prototype structure.

  9. Active sites in char gasification. Quarterly technical progress report, 1 January 1984-31 March 1984. [Polymers of phenol-formaldehyde family; chars produced from model compounds

    Energy Technology Data Exchange (ETDEWEB)

    Calo, J.M.; Suubers, E.M.; Wojtowicz, M.; Lilly, W.

    1984-05-01

    This project is concerned with the study of the nature and behavior of active sites in gasification of chars produced from synthesized model compounds, primarily of the phenol-formaldehyde family of resins. The current technical progress report presents further developments on resin synthesis and characterization and the design of a pyro-gasifier reactor for transient kinetic studies of the chars produced from the model compounds. 7 references, 12 figures, 2 tables.

  10. Effects of periodic desiccation on the synthesis of the UV-screening compound, scytonemin, in cyanobacteria.

    Science.gov (United States)

    Fleming, Erich D; Castenholz, Richard W

    2007-06-01

    Scytonemin is an ultraviolet radiation (UVR)-screening compound synthesized by some sheathed cyanobacteria exposed to high solar and sky radiation. It is primarily produced in response to UVA radiation, but certain environmental stresses can enhance synthesis. This study focuses on the effects of periodic desiccation on scytonemin synthesis in three desiccation-tolerant cyanobacterial strains, Nostoc punctiforme PCC 73102, Chroococcidiopsis CCMEE 5056 and Chroococcidiopsis CCMEE 246. Nostoc punctiforme and Chroococcidiopsis CCMEE 5056 exposed to UVA radiation produced more concentrated scytonemin screens when experiencing periodic desiccation (i.e. 1 day desiccated for every 2 days hydrated) than when continuously hydrated. A more concentrated scytonemin screen would reduce the amount of UVR damage accrued when cells are desiccated and metabolically inactive. This might allow the cyanobacteria to allocate more energy to systems other than UVR damage repair during rehydration, which would facilitate recovery. The scytonemin screen is extremely stable, remaining largely intact in the sheaths of desiccated N. punctiforme even when continuously exposed to UVA radiation for about 2 months. In contrast to the above findings, scytonemin synthesis in Chroococcidiopsis CCMEE 246, a strain that produces scytonemin constitutively under low visible light (no UVA), was partially inhibited by periodic desiccation.

  11. Towards a national report card in nursing: a knowledge synthesis.

    Science.gov (United States)

    Doran, Diane; Mildon, Barbara; Clarke, Sean

    2011-06-01

    This paper is an abridged version of a knowledge synthesis undertaken to inform the proceedings of a collaborative forum of nurse leaders convened under the auspices of Health Canada, the Academy of Canadian Executive Nurses, the Canadian Nurses Association and Canada Health Infoway for the purpose of discussing the development of a nursing report card for Canada. The synthesis summarized the state of the science in the measurement of nursing-sensitive outcomes and the utilization of nursing report cards - information that informed forum participants' dialogue and planning. This condensed version of the synthesis focuses on initiatives related to outcomes and performance monitoring in nursing, including specific indicators and reporting systems and the development, implementation and utilization of nursing report cards.

  12. Enhancing transparency in reporting the synthesis of qualitative research: ENTREQ

    Science.gov (United States)

    2012-01-01

    Background The syntheses of multiple qualitative studies can pull together data across different contexts, generate new theoretical or conceptual models, identify research gaps, and provide evidence for the development, implementation and evaluation of health interventions. This study aims to develop a framework for reporting the synthesis of qualitative health research. Methods We conducted a comprehensive search for guidance and reviews relevant to the synthesis of qualitative research, methodology papers, and published syntheses of qualitative health research in MEDLINE, Embase, CINAHL and relevant organisational websites to May 2011. Initial items were generated inductively from guides to synthesizing qualitative health research. The preliminary checklist was piloted against forty published syntheses of qualitative research, purposively selected to capture a range of year of publication, methods and methodologies, and health topics. We removed items that were duplicated, impractical to assess, and rephrased items for clarity. Results The Enhancing transparency in reporting the synthesis of qualitative research (ENTREQ) statement consists of 21 items grouped into five main domains: introduction, methods and methodology, literature search and selection, appraisal, and synthesis of findings. Conclusions The ENTREQ statement can help researchers to report the stages most commonly associated with the synthesis of qualitative health research: searching and selecting qualitative research, quality appraisal, and methods for synthesising qualitative findings. The synthesis of qualitative research is an expanding and evolving methodological area and we would value feedback from all stakeholders for the continued development and extension of the ENTREQ statement. PMID:23185978

  13. Ionic liquids as an electrolyte for the electro synthesis of organic compounds.

    Science.gov (United States)

    Kathiresan, Murugavel; Velayutham, David

    2015-12-25

    The use of ionic liquids (ILs) as a solvent and an electrolyte for electro organic synthesis has been reviewed. To date several ILs exist, however the ILs based on tetraalkylammonium, pyrrolidinium, piperidinium and imidazolium cations with BF4(-), PF6(-), and TFSI anions have been widely used and explored the most. Electro organic synthesis in ionic liquid media leading to the synthesis of a wide range of organic compounds has been discussed. Anodic oxidation or cathodic reduction will generate radical cation or anion intermediates, respectively. These radicals can undergo self coupling or coupling with other molecules yielding organic compounds of interest. The cation of the IL is known to stabilize the radical anion extensively. This stabilization effect has a specific impact on the electrochemical CO2 reduction and coupling to various organics. The relative stability of the intermediates in IL leads to the formation of specific products in higher yields. Electrochemical reduction of imidazolium or thiazolium based ILs generates N-heterocyclic carbenes that have been shown to catalyze a wide range of base or nucleophile catalyzed organic reactions in IL media, an aspect that falls into the category of organocatalysis. Electrochemical fluorination or selective electrochemical fluorination is another fascinating area that delivers selectively fluorinated organic products in Et3N·nHF or Et4NF·nHF adducts (IL) via anodic oxidation. Oxidative polymerization in ILs has been explored the most; although morphological changes were observed compared to the conventional methods, polymers were obtained in good yields and in some cases ILs were used as dopants to improve the desired properties.

  14. Synthesis and characterisation of Copper Zinc Tin Sulphide (CZTS) compound for absorber material in solar-cells

    Science.gov (United States)

    Kheraj, Vipul; Patel, K. K.; Patel, S. J.; Shah, D. V.

    2013-01-01

    The development of thin-film semiconductor compounds, such as Copper Indium Gallium Selenide (CIGS), has caused remarkable progress in the field of thin-film photovoltaics. However, the scarcity and the increasing prices of indium impose the hunt for alternative materials. The Copper Zinc Tin Sulphide (CZTS) is one of the promising emerging materials with Kesterite-type crystal structure and favourable material properties like high absorption co-efficient and direct band-gap. Moreover, all the constituent elements of CZTS are non-toxic and aplenty on the earth-crust, making it a potential candidate for the thin-film photovoltaics. Here we report the synthesis of CZTS powder from its constituent elements, viz. copper, zinc, tin and sulphur, in an evacuated Quartz ampoule at 1030 K temperature. The sulphur content in the raw mixture in the ampoule was varied and optimised in order to attain the desired atomic stoichiometry of the compound. The synthesised powder was characterised by X-Ray diffraction technique (XRD), Raman Scattering Spectroscopy, Energy Dispersive Analysis of X-Ray (EDAX) and UV-Visible Absorption Spectra. The XRD Patterns of the synthesised compound show the preferred orientation of (112), (220) and (312) planes, confirming the Kesterite structure of CZTS. The chemical composition of the powder was analysed by EDAX and shows good atomic stoichiometry of the constituent elements in the CZTS compound. The UV-Vis absorption spectra confirm the direct band-gap of about 1.45 eV, which is quite close to the optimum value for the semiconductor material as an absorber in solar-cells.

  15. Synthesis and Antiplatelet Activity of Antithrombotic Thiourea Compounds: Biological and Structure-Activity Relationship Studies

    Directory of Open Access Journals (Sweden)

    André Luiz Lourenço

    2015-04-01

    Full Text Available The incidence of hematological disorders has increased steadily in Western countries despite the advances in drug development. The high expression of the multi-resistance protein 4 in patients with transitory aspirin resistance, points to the importance of finding new molecules, including those that are not affected by these proteins. In this work, we describe the synthesis and biological evaluation of a series of N,N'-disubstituted thioureas derivatives using in vitro and in silico approaches. New designed compounds inhibit the arachidonic acid pathway in human platelets. The most active thioureas (compounds 3d, 3i, 3m and 3p displayed IC50 values ranging from 29 to 84 µM with direct influence over in vitro PGE2 and TXA2 formation. In silico evaluation of these compounds suggests that direct blockage of the tyrosyl-radical at the COX-1 active site is achieved by strong hydrophobic contacts as well as electrostatic interactions. A low toxicity profile of this series was observed through hemolytic, genotoxic and mutagenic assays. The most active thioureas were able to reduce both PGE2 and TXB2 production in human platelets, suggesting a direct inhibition of COX-1. These results reinforce their promising profile as lead antiplatelet agents for further in vivo experimental investigations.

  16. Methods for chemical synthesis of biologically active compounds using supramolecular protective groups and novel compounds obtainable Thereby

    NARCIS (Netherlands)

    HERRMANN, ANDREAS; BASTIAN ANDREAS, ALEXANDER; MARCOZZI, ALESSIO

    2014-01-01

    The invention relates to drug development and synthetic chemistry, in particular to the manufacture of biologically active compounds based on naturally occurring molecules. It also relates to novel biologically active compounds, for example aminoglycoside antibiotics, in a substantially pure

  17. The Synthesis and Evaluation of Third-Order Optical Nonlinearities of Model Compounds Containing Benzothiazole, Benzimidazole and Benzoxazole Moieties.

    Science.gov (United States)

    1991-02-01

    AD-A235 622 WL-TR-91-4015 THE SYNTHESIS AND EVALUATION OF THIRD-ORDER OPTICAL NONLINEARITIES OF MODEL COMPOUNDS CONTAINING BENZOTHIAZOLE ...Nonlinearities of Model Compounds Containing Benzothiazole , Benzimidazole, and Benzoxazole Moieties 12 PERSONAL AUTHOR(S) Bruce A. Reinhardt, Marilyn R...necessary and identify by block number) FIELD GROUP SUB-GROUP nonlinear optical properties benzothiazole u/ 03 degenerate four-wave mixing benzimidazole 21

  18. Synthesis of TiO2 nanocrystals with a high affinity for amine organic compounds.

    Science.gov (United States)

    Gonçalves, Ricardo H; Schreiner, Wido Herwig; Leite, Edson R

    2010-07-20

    This article describes a different approach to the colloidal synthesis of TiO(2) nanocrystals using a polymer melt as a solvent. This approach allowed us to obtain a colloidal dispersion with a high degree of stability in a polymeric solvent, resulting in a transparent colloid. Using this method, it was possible to obtain the TiO(2) nanocrystal with Brønsted acid sites and polymer chains chemically anchored on the nanocrystal surface. The acid surface of those nanocrystals has the chemical property to react in the presence of amine organic compounds and to maintain the colloidal stability. In this way, TiO(2) nanocrystals were combined with a molecular probe containing amine functional groups such as polyaniline. Through the combination of the molecular probe and inorganic nanocrystals, we obtained a hybrid material with interesting chemical, optical, and electronic behavior, making it a promising material for photovoltaic, photochromic, and sensor devices.

  19. Synthesis of Graphene Oxide by Oxidation of Graphite with Ferrate(VI) Compounds: Myth or Reality?

    Science.gov (United States)

    Sofer, Zdeněk; Luxa, Jan; Jankovský, Ondřej; Sedmidubský, David; Bystroň, Tomáš; Pumera, Martin

    2016-09-19

    It is well established that graphene oxide can be prepared by the oxidation of graphite using permanganate or chlorate in an acidic environment. Recently, however, the synthesis of graphene oxide using potassium ferrate(VI) ions has been reported. Herein, we critically replicate and evaluate this new ferrate(VI) oxidation method. In addition, we test the use of potassium ferrate(VI) for the synthesis of graphene oxide under various experimental routes. The synthesized materials are analyzed by a number of analytical methods in order to confirm or disprove the possibility of synthesizing graphene oxide by the ferrate(VI) oxidation route. Our results confirm the unsuitability of using ferrate(VI) for the oxidation of graphite on graphene oxide because of its high instability in an acidic environment and low oxidation power in neutral and alkaline environments.

  20. Synthesis and purification of some main group organometallic precursors for compound semiconductors

    Indian Academy of Sciences (India)

    Vimal K Jain

    2005-07-01

    Metal–organic vapour phase epitaxy/chemical vapour deposition (MOVPE/MOCVD) has emerged recently as the method of choice for large scale preparation of a variety of low dimension inorganic materials; particularly compound semiconductors, used in modern electronic and opto-electronic devices. The success of this process depends on the availability of suitable molecular precursors of desired purity. Group V hydrides (e.g. NH3, PH3, AsH3, SbH3) have been employed conventionally for deposition of III–V semiconductor materials. Inherent weakness of this hydride source, particularly heavier ones (for instance very low utilization (> 0.1%) of AsH3 in GaAs synthesis; ∼ 4 h half life of SbH3 at room temperature) has been a driving force to develop new molecular precursors with desirable properties. This talk will briefly review synthesis and purification of several precursors of groups III (Ga, In), IV, V (As, Sb) and VI (Se, Te).

  1. Multigram Synthesis and in Vivo Efficacy Studies of a Novel Multitarget Anti-Alzheimer’s Compound

    Directory of Open Access Journals (Sweden)

    Irene Sola

    2015-03-01

    Full Text Available We describe the multigram synthesis and in vivo efficacy studies of a donepezil‒huprine hybrid that has been found to display a promising in vitro multitarget profile of interest for the treatment of Alzheimer’s disease (AD. Its synthesis features as the key step a novel multigram preparative chromatographic resolution of intermediate racemic huprine Y by chiral HPLC. Administration of this compound to transgenic CL4176 and CL2006 Caenorhabditis elegans strains expressing human Aβ42, here used as simplified animal models of AD, led to a significant protection from the toxicity induced by Aβ42. However, this protective effect was not accompanied, in CL2006 worms, by a reduction of amyloid deposits. Oral administration for 3 months to transgenic APPSL mice, a well-established animal model of AD, improved short-term memory, but did not alter brain levels of Aβ peptides nor cortical and hippocampal amyloid plaque load. Despite the clear protective and cognitive effects of AVCRI104P4, the lack of Aβ lowering effect in vivo might be related to its lower in vitro potency toward Aβ aggregation and formation as compared with its higher anticholinesterase activities. Further lead optimization in this series should thus focus on improving the anti-amyloid/anticholinesterase activity ratio.

  2. Synthesis and Antiplasmodial Activity of 2-(4-Methoxyphenyl-4-Phenyl-1,10-Phenanthroline Derivative Compounds

    Directory of Open Access Journals (Sweden)

    Nazudin

    2012-08-01

    Full Text Available A unique of synthetic methods was employed to prepare 2-(4-methoxyphenyl-4-phenyl-1,10-phenanthroline (5 derivatives from 4-methoxy-benzaldehyde (1, acetophenone (2, and 8-aminoquinoline (4 with aldol condensation and cyclization reactions. The derivatives were tested through antiplasmodial test. The synthesis of derivatives compound 5 was conducted in three steps. The 3-(4-methoxyphenyl-1-phenylpropenone 3 was synthesized through aldol condensation of 1 and 2 which has a yield of 96.42%. The compound 5 was synthesized through cyclization of compound 4 and 3 with 84.55% yield. The derivative of compound 5 was synthesized from compound 5 using DMS and DES reagents which refluxed for 21 and 22 h, to produce (1-N-methyl-9-(4-methoxyphenyl-7-phenyl-1,10-phenanthrolinium sulfate (6 and (1-N-ethyl-9-(4-methoxyphenyl-7-phenyl-1,10-phenanthrolinium sulfate (7 with 91.42 and 86.36% yields, respectively. Results of in vitro testing of antiplasmodial activity of compound 5 derivatives (i.e., compound 6 and 7 against chloroquine-resistant P. falciparum FCR3 strain showed that compound 7 had higher antimalarial activity than compounds 5 and 6. Whereas, results of in vitro testing against chloroquine-sensitive P. falciparum D10 strain showed that compound 6 has higher antimalarial activity than compounds 5 and 7.

  3. Green Synthesis and Regioselective Control of Sn/I2 Mediated Allylation of Carbonyl Compounds with Crotyl Halide in Water

    Institute of Scientific and Technical Information of China (English)

    ZHANG,Yan; ZHA,Zhang-Gen; ZHOU,Yu-Qing; WANG,Zhi-Yong

    2004-01-01

    @@ Barbier-type carbonyl allylation is particularly useful due to ease of operation and the availability and tractability of allylic substrates,[1] Metals such as indium, zinc and tin are often used as the mediator. Here we present a green approach toward the synthesis, that is, Sn/I2 mediated allylation of carbonyl compounds with crotyl halide in water.

  4. Photochemical Synthesis and Ligand Exchange Reactions of Ru(CO)[subscript 4] (Eta[superscript 2]-Alkene) Compounds

    Science.gov (United States)

    Cooke, Jason; Berry, David E.; Fawkes, Kelli L.

    2007-01-01

    The photochemical synthesis and subsequent ligand exchange reactions of Ru(CO)[subscript 4] (eta[superscript2]-alkene) compounds has provided a novel experiment for upper-level inorganic chemistry laboratory courses. The experiment is designed to provide a system in which the changing electronic properties of the alkene ligands could be easily…

  5. Combinatorial Synthesis and Discovery of an Antibiotic Compound. An Experiment Suitable for High School and Undergraduate Laboratories

    Science.gov (United States)

    Wolkenberg, Scott E.; Su, Andrew I.

    2001-06-01

    An exercise demonstrating solution-phase combinatorial chemistry and its application to drug discovery is described. The experiment involves the synthesis of six libraries of three hydrazones, screening the libraries for antibiotic activity, and deconvolution to determine the active individual compound. The laboratory was designed for a high school classroom, though it can easily be expanded to suit a college introductory organic laboratory course.

  6. Synthesis, Structure and Antitumour Properties of a New 1,2-Propylenediaminetetraacetate-Ruthenium(III) Compound.

    Science.gov (United States)

    Vilaplana, R; Romero, M A; Quirós, M; Salas, J M; González-Vílchez, F

    1995-01-01

    A novel complex formed by ruthenium (III) and the sequestering ligand 1,2-propylenediaminetetraacetic acid (PDTA) has been synthetized and characterized. The structure of the monomeric compound, studied by X-ray diffraction , shows an almost symmetric octahedral geometry around the metal ion, with two chlorine atoms in a cis conformation. The antitumour activity against a variety of murine and human cancers is reported.

  7. Survey of electrochemical production of inorganic compounds. Final report

    Energy Technology Data Exchange (ETDEWEB)

    1980-10-01

    The electrochemical generation of inorganic compounds, excluding chlorine/caustic, has been critically reviewed. About 60 x 10/sup 12/ Btu/y fossil fuel equivalent will be used in the year 2000 for the electrosynthesis of inorganic compounds. Significant energy savings in chlorate production can result from the development of suitable electrocatalysts for lowering the cathodic overpotential. Perchlorates, electrolytic hypochlorite, electrolytic manganese dioxide, fluorine and other miscellaneous compounds use relatively small amounts of electrical energy. Implementation of caustic scrubber technology for stack gas cleanup would result in appreciable amounts of sodium sulfate which could be electrolyzed to regenerate caustic. Hydrogen peroxide, now produced by the alkyl anthraquinone process, could be made electrolytically by a new process coupling anodic oxidation of sulfate with cathodic reduction of oxygen in alkaline solution. Ozone is currently manufactured using energy-inefficient silent discharge equipment. A novel energy-efficient approach which uses an oxygen-enhanced anodic reaction is examined.

  8. Synthesis of national reports for Rio+20

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2013-01-15

    In the lead up to the United Nations Conference on Sustainable Development (Rio+20), which took place in Brazil in June 2012, there were numerous efforts in countries around the world to help governments, civil society organizations and individuals prepare for the event. One of the more significant efforts led by UNDP in collaboration with the United Nations Department of Economic and Social Affairs (UN DESA) was a support programme to 72 countries across all regions to build a consensus on national views around the themes and objectives of the Rio+20 Conference. This report highlights significant advances in sustainable development from almost 60 country reports and underscores the challenges and bottlenecks to moving beyond the economic-led growth strategies of the past 20 years.

  9. [Compound odontoma with history of trauma: report of a case].

    Science.gov (United States)

    Sámano Iturría, G; Cedeño Pacheco, E

    1988-08-01

    Clinical and roentgenographical features are described for a compound odontoma in a ten-year old male with a history of trauma in the anterior region of the face. Diagnostical methods and surgical handling are discussed, with a review of the pertinent literature.

  10. Synthesis report on thermally driven coupled processes

    Energy Technology Data Exchange (ETDEWEB)

    Hardin, E.L.

    1997-10-15

    The main purpose of this report is to document observations and data on thermally coupled processes for conditions that are expected to occur within and around a repository at Yucca Mountain. Some attempt is made to summarize values of properties (e.g., thermal properties, hydrologic properties) that can be measured in the laboratory on intact samples of the rock matrix. Variation of these properties with temperature, or with conditions likely to be encountered at elevated temperature in the host rock, is of particular interest. However, the main emphasis of this report is on direct observation of thermally coupled processes at various scales. Direct phenomenological observations are vitally important in developing and testing conceptual models. If the mathematical implementation of a conceptual model predicts a consequence that is not observed, either (1) the parameters or the boundary conditions used in the calculation are incorrect or (2) the conceptual basis of the model does not fit the experiment; in either case, the model must be revised. For example, the effective continuum model that has been used in thermohydrology studies combines matrix and fracture flow in a way that is equivalent to an assumption that water is imbibed instantaneously from fractures into adjacent, partially saturated matrix. Based on this approximation, the continuum-flow response that is analogous to fracture flow will not occur until the effective continuum is almost completely saturated. This approximation is not entirely consistent with some of the experimental data presented in this report. This report documents laboratory work and field studies undertaken in FY96 and FY97 to investigate thermally coupled processes such as heat pipes and fracture-matrix coupling. In addition, relevant activities from past years, and work undertaken outside the Yucca Mountain project are summarized and discussed. Natural and artificial analogs are also discussed to provide a convenient source of

  11. Synthesis, double-helix formation, and higher-assembly formation of chiral polycyclic aromatic compounds: conceptual development of polyketide aldol synthesis.

    Science.gov (United States)

    Yamaguchi, Masahiko; Shigeno, Masanori; Saito, Nozomi; Yamamoto, Koji

    2014-02-01

    Polycyclic aromatic compounds are an important group of substances in chemistry, and the study of their properties is a subject of interest in the development of drugs and materials. We have been conducting studies to develop chiral polycyclic aromatic compounds, i.e., helicenes and equatorenes. These helical molecules showed notable aggregate-forming properties and the capability for chiral recognition exerted by noncovalent bond interactions, which were not observed in compounds with central chirality. Homo- and hetero-double-helix-forming helicene oligomers were developed, and the latter self-assembled to form gels and vesicles. In this article, we describe such hierarchical studies of polycyclic aromatic compounds, which were started from polyketide aldol synthesis.

  12. Synthesis Organonitrogen Compounds from Patchouli Alcohol Through Ritter Reaction with Acetonitrile and Its Toxicity to Artemia salina Leach.

    Directory of Open Access Journals (Sweden)

    Khoirun Nisyak

    2013-03-01

    Full Text Available Patchouli oil contains a compound with biological activities to human body called the patchouli alcohol that can be further developed in medical field. This research aimed to synthesize organonitrogen compound from patchouli alcohol through Ritter reaction with acetonitrile and discover its toxicity towards Artemia salina Leach. The isolation of patchouli alcohol from patchouli oil using fractional distillation under reduced pressure method. The synthesis of organonitrogen compound is done at room temperature with the mol ratio of patchouli alcohol: acetonitrile: sulfuric acid is 1:1,5:4 for 24 hours. The result showed that the amount of patchouli alcohol produced from fractional distillation is 65,25%. The main product yielded from the synthesis between patchouli alcohol and acetonitrile through Ritter reaction is 36,93 % of N-(4,8a,9,9-tetramethyl decahydro-1,6-methanonaphtalene-1-yl acetamide. Starting material used have LC50 of 77,39 ppm. The product of synthesis have higher toxicity level than starting material, which have LC50 value is 10,39 ppm with the potential as medical compounds.

  13. First Total Synthesis of 4,5-Secoeudesmane-type and Iphionane-type Compounds- Synthesis of 4,5-Dioxo-seco-γ-eudesmol and 5β ,11-Dihydroxyiphionan-4-one

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    @@ 4, 5-Secoeudesmane-type and iphionane-type compounds are sesquiterpenes with new carbon skeletons found in natrual sources in recent years.1-6 The co-occurence of 4, 5-secoeudesmanes, iphionanes and eudesmanes as natrual products suggests that 4, 5-secoeudesmanes, iphionanes most likely are generated biogenetically from eudesmanes, and iphionanes are formed biogenetically by aldol reaction of 4, 5-dioxosecoeudesmanes1,4,6,7. The study on the synthesis of this two kind of new sesquiterpenes has not been reported in the literature.

  14. Identification, synthesis, and characterization of novel sulfur-containing volatile compounds from the in-depth analysis of Lisbon lemon peels (Citrus limon L. Burm. f. cv. Lisbon).

    Science.gov (United States)

    Cannon, Robert J; Kazimierski, Arkadiusz; Curto, Nicole L; Li, Jing; Trinnaman, Laurence; Jańczuk, Adam J; Agyemang, David; Da Costa, Neil C; Chen, Michael Z

    2015-02-25

    Lemons (Citrus limon) are a desirable citrus fruit grown and used globally in a wide range of applications. The main constituents of this sour-tasting fruit have been well quantitated and characterized. However, additional research is still necessary to better understand the trace volatile compounds that may contribute to the overall aroma of the fruit. In this study, Lisbon lemons (C. limon L. Burm. f. cv. Lisbon) were purchased from a grove in California, USA, and extracted by liquid-liquid extraction. Fractionation and multidimensional gas chromatography-mass spectrometry were utilized to separate, focus, and enhance unidentified compounds. In addition, these methods were employed to more accurately assign flavor dilution factors by aroma extract dilution analysis. Numerous compounds were identified for the first time in lemons, including a series of branched aliphatic aldehydes and several novel sulfur-containing structures. Rarely reported in citrus peels, sulfur compounds are known to contribute significantly to the aroma profile of the fruit and were found to be aroma-active in this particular study on lemons. This paper discusses the identification, synthesis, and organoleptic properties of these novel volatile sulfur compounds.

  15. Synthesis, crystal structure and high-temperature transport properties of the new cluster compound Rb2Mo15Se19

    Science.gov (United States)

    Daigre, Gilles; Gougeon, Patrick; Gall, Philippe; Gautier, Régis; Guillou, Olivier; Vaney, Jean-Baptiste; Candolfi, Christophe; Dauscher, Anne; Lenoir, Bertrand

    2016-05-01

    We report on the synthesis, crystal structure and high-temperature transport properties of Rb2Mo15Se19, a new member of the large family of M2Mo15Se19 (M=In, Tl, K, Ba) cluster compounds. Polycrystalline samples and single crystals of the ternary selenide Rb2Mo15Se19 were obtained by solid-state reactions. The trigonal crystal structure, successfully refined in space group R 3 bar c (No. 167) with unit-cell parameters a=9.7618(1) Å, c=58.254(1) Å and Z=6, was determined by single-crystal X-ray diffraction. The crystal structure contains Mo6 Se8i Se6a and Mo9Se11iSe6a cluster units in equal proportion and separated from each other by large voids, which are filled up by Rb atoms. Measurements of the electrical resistivity, thermopower and thermal conductivity revealed that Rb2Mo15Se19 behaves as a p-type metal with relatively low electrical resistivity and thermopower. Despite its complex crystal structure, the lattice thermal conductivity that amounts to 1.3 W m-1 K-1 at 300 K is significantly higher than in Ag-filled analogues, which provides possible guidelines to enhance its thermoelectric properties.

  16. High molecule compound synthesis from carbon dioxide; Nisanka tanso karano kobunshi gosei

    Energy Technology Data Exchange (ETDEWEB)

    Mishima, K. [Fukuoka Univ., Fukuoka (Japan)

    2000-09-05

    Recently, synthesis of organic substances and high molecule compounds using carbon dioxide of liquid or supercritical state as raw material is paid attention so as the influential means to realize the green chemistry. A zinc based catalyst which could synthesize the activated copolymer from oxidized cyclohexane and carbon dioxide was developed by Coates, Beckman et al. The high-activated fluoridation zinc based catalyst which dissolved the high-pressure carbon dioxide was developed by Beckman, etc. The possibility of the manufacturing of the high molecule copolymer which is made from carbon dioxide and oxidized cyclohexane as a raw material was shown by an appearance of this catalyst. In addition, a synthesizing method of lactone from carbon dioxide and olefinic hydrocarbon is being examined by Beckman. If this method is used practically, the manufacturing of a gentle biodegradable polymer in the environment which is made from carbon dioxide as a raw material becomes also possible. However, adequate catalysts are necessary so that this reaction may progress. (NEDO)

  17. The atmosphere of the primitive earth and the prebiotic synthesis of organic compounds

    Science.gov (United States)

    Miller, S. L.; Schlesinger, G.

    1983-01-01

    The prebiotic synthesis of organic compounds is investigated using a spark discharge on various simulated prebiotic atmospheres at 25 C. It is found that glycine is almost the only amino acid produced from the model atmospheres containing CO and CO2. These results show that the maximum yield is about the same for the three carbon sources (CO, CO2, and CH4) at high H2/carbon ratios, but that CH4 is superior at low H2/carbon ratios. CH4 is found to yield a much greater variety of amino acids than either CO or CO2. If it is assumed that amino acids more complex than glycine were required for the origin of life, then these findings indicate the need for CH4 in the primitive atmosphere. The yields of cyanide and formaldehyde are shown to parallel the amino acid results, with yields of HCN and H2CO as high as 13 percent based on carbon. Ammonia is also found to be produced from N2 in experiments with no added NH3 in yields as high as 4.9 percent. These results indicate that large amounts of NH3 would have been synthesized on the primitive earth by electric discharges.

  18. Synthesis of heterometallic compounds with uncommon combinations of elements for oxide nanomaterials using organometallics.

    Science.gov (United States)

    John, Łukasz; Sobota, Piotr

    2014-02-18

    Oxide nanomaterials with interesting electronic and magnetic properties have applications including superconductors, magnetic core materials, high-frequency devices, and gas sensors. They can also serve as efficient oxide lattices for luminescent ions. Highly phase-pure BaHfO3 nanopowders are extremely desirable as matrices for luminescent doping, and barium hafnate is an attractive host lattice for new X-ray phosphors, which are much more effective than the phosphors currently used in radiology and computed tomography. This wide range of applications creates a strong impetus for novel and inexpensive methods for their synthesis. Classically, mixed-cation oxide ceramics are synthesized according to conventional solid-state reactions involving oxides, carbonates, or nitrates at relatively high temperatures (∼1500 °C). These procedures are inefficient and often lead to inhomogeneous by-products and poor control over the stoichiometry and phase purity. Among the new preparation techniques are those involving metal alkoxides and aryloxides with strictly defined metal stoichiometries at the molecular level. In this Account, we describe several structurally interesting heterometallic alkoxoorganometallic compounds prepared via reactions of organometallic compounds (MMe3 where M = Al, In, Ga) with group 2 alkoxides having additional protonated hydroxyl group(s) in the alcohol molecule present in the metal coordination sphere. Using lower temperatures than in the conventional solid-state thermal routes involving carbonate/oxide mixtures, we can easily transform these new complexes, with rarely found combinations of metallic precursors (Ba/In, Sr/Al, and Ba/Ga), into highly pure binary oxide materials that can be used, in a similar manner to perovskites and spinels, as host matrices for various lanthanide ions. Furthermore, our studies on titanium, zirconium, and hafnium metallocenes showed them to be attractive and cheap precursors for an extensive range of novel

  19. A synthesis of parameters related to the binding of neutral organic compounds to charcoal.

    Science.gov (United States)

    Hale, Sarah E; Arp, Hans Peter H; Kupryianchyk, Darya; Cornelissen, Gerard

    2016-02-01

    The sorption strength of neutral organic compounds to charcoal, also called biochar was reviewed and related to charcoal and compound properties. From 29 studies, 507 individual Freundlich sorption coefficients were compiled that covered the sorption strength of 107 organic contaminants. These sorption coefficients were converted into charcoal-water distribution coefficients (K(D)) at aqueous concentrations of 1 ng/L, 1 µg/L and 1 mg/L. Reported log K(D) values at 1 µg/L varied from 0.38 to 8.25 across all data. Variation was also observed within the compound classes; pesticides, herbicides and insecticides, PAHs, phthalates, halogenated organics, small organics, alcohols and PCBs. Five commonly reported variables; charcoal production temperature T, surface area SA, H/C and O/C ratios and organic compound octanol-water partitioning coefficient, were correlated with KD values using single and multiple-parameter linear regressions. The sorption strength of organic compounds to charcoals increased with increasing charcoal production temperature T, charcoal SA and organic pollutant octanol-water partitioning coefficient and decreased with increasing charcoal O/C ratio and charcoal H/C ratio. T was found to be correlated with SA (r(2) = 0.66) and O/C (r(2) = 0.50), particularly for charcoals produced from wood feedstocks (r(2) = 0.73 and 0.80, respectively). The resulting regression: log K(D)=(0.18 ± 0.06) log K(ow) + (5.74 ± 1.40) log T + (0.85 ± 0.15) log SA + (1.60 ± 0.29) log OC + (-0.89 ± 0.20) log HC + (-13.20 ± 3.69), r(2) = 0.60, root mean squared error = 0.95, n = 151 was obtained for all variables. This information can be used as an initial screening to identify charcoals for contaminated soil and sediment remediation. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. The Emissions Gap Report 2014:A UNEP Synthesis Report

    OpenAIRE

    Farrell, Timothy Clifford

    2014-01-01

    This fifth Emissions Gap report has a different focus from previous years. While it updates the 2020 emissions gap analysis, it gives particular attention to the implications of the global carbon dioxide emissions budget for staying within the 2 °C limit beyond 2020. It does so because countries are giving increasing attention to where they need to be in 2025, 2030 and beyond. Furthermore, this year’s update of the report benefits from the findings on the emissions budget from the latest seri...

  1. Tools for Chemical Biology: New Macrocyclic Compounds from Diversity-Oriented Synthesis and Toward Materials from Silver(I) Acetylides

    DEFF Research Database (Denmark)

    Madsen, Charlotte Marie

    Part I The formation of a library of diverse macrocyclic compounds with different functionalities and ring sizes in a few steps from two easily accessible α,ω-diol building blocks is presented. The building blocks are combined by esteriffcations in four different ways leading to the formation of ...... of uoro-iodoadamantanes. However, overall the results provide a good starting point for the synthesis of new triptycene and adamantane-containing molecules that can interact with carbon nanotubes....

  2. Palladium- and copper-mediated N-aryl bond formation reactions for the synthesis of biological active compounds

    Directory of Open Access Journals (Sweden)

    Burkhard Koenig

    2011-01-01

    Full Text Available N-Arylated aliphatic and aromatic amines are important substituents in many biologically active compounds. In the last few years, transition-metal-mediated N-aryl bond formation has become a standard procedure for the introduction of amines into aromatic systems. While N-arylation of simple aromatic halides by simple amines works with many of the described methods in high yield, the reactions may require detailed optimization if applied to the synthesis of complex molecules with additional functional groups, such as natural products or drugs. We discuss and compare in this review the three main N-arylation methods in their application to the synthesis of biologically active compounds: Palladium-catalysed Buchwald–Hartwig-type reactions, copper-mediated Ullmann-type and Chan–Lam-type N-arylation reactions. The discussed examples show that palladium-catalysed reactions are favoured for large-scale applications and tolerate sterically demanding substituents on the coupling partners better than Chan–Lam reactions. Chan–Lam N-arylations are particularly mild and do not require additional ligands, which facilitates the work-up. However, reaction times can be very long. Ullmann- and Buchwald–Hartwig-type methods have been used in intramolecular reactions, giving access to complex ring structures. All three N-arylation methods have specific advantages and disadvantages that should be considered when selecting the reaction conditions for a desired C–N bond formation in the course of a total synthesis or drug synthesis.

  3. Vapor phase synthesis of compound semiconductors, from thin films to nanoparticles

    Science.gov (United States)

    Sarigiannis, Demetrius

    A counterflow jet reactor was developed to study the gas-phase decomposition kinetics of organometallics used in the vapor phase synthesis of compound semiconductors. The reactor minimized wall effects by generating a reaction zone near the stagnation point of two vertically opposed counterflowing jets. Smoke tracing experiments were used to confirm the stability of the flow field and validate the proposed heat, mass and flow models of the counterflow jet reactor. Transport experiments using ethyl acetate confirmed the overall mass balance for the system and verified the ability of the model to predict concentrations at various points in the reactor under different flow conditions. Preliminary kinetic experiments were performed with ethyl acetate and indicated a need to redesign the reactor. The counterflow jet reactor was adapted for the synthesis of ZnSe nanoparticles. Hydrogen selenide was introduced through one jet and dimethylzinc-triethylamine through the other. The two precursors reacted in a region near the stagnation zone and polycrystalline particles of zinc selenide were reproducibly synthesized at room temperature and collected for analysis. Raman spectroscopy confirmed that the particles were crystalline zinc selenide, Morphological analysis using SEM clearly showed the presence of aggregates of particles, 40 to 60 nanometers in diameter. Analysis by TEM showed that the particles were polycrystalline in nature and composed of smaller single crystalline nanocrystallites, five to ten nanometers in diameter. The particles in the aggregate had the appearance of being sintered together. To prevent this sintering, a split inlet lower jet was designed to introduce dimethylzinc through the inner tube and a surface passivator through the outer one. This passivating agent appeared to prevent the particles from agglomerating. An existing MOVPE reactor for II-VI thin film growth was modified to grow III-V semiconductors. A novel new heater was designed and built

  4. Studies on Synthesis and Biological Activities of Novel Triazole Compounds Containing 1,3-Dioxolane

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Nine title compounds were synthesized. Their strucures were identified by means of IR, EA, 1H NMR and MS. The results from the primary biological test show that all the compounds have some activitiies of fungicide and plant growth regulator. When R group is 2,4-Cl2C6H3, compound 2 or compound 4 shows better biological activities.

  5. Optimized Solid Phase-Assisted Synthesis of Dendrons Applicable as Scaffolds for Radiolabeled Bioactive Multivalent Compounds Intended for Molecular Imaging

    Directory of Open Access Journals (Sweden)

    Gabriel Fischer

    2014-05-01

    Full Text Available Dendritic structures, being highly homogeneous and symmetric, represent ideal scaffolds for the multimerization of bioactive molecules and thus enable the synthesis of compounds of high valency which are e.g., applicable in radiolabeled form as multivalent radiotracers for in vivo imaging. As the commonly applied solution phase synthesis of dendritic scaffolds is cumbersome and time-consuming, a synthesis strategy was developed that allows for the efficient assembly of acid amide bond-based highly modular dendrons on solid support via standard Fmoc solid phase peptide synthesis protocols. The obtained dendritic structures comprised up to 16 maleimide functionalities and were derivatized on solid support with the chelating agent DOTA. The functionalized dendrons furthermore could be efficiently reacted with structurally variable model thiol-bearing bioactive molecules via click chemistry and finally radiolabeled with 68Ga. Thus, this solid phase-assisted dendron synthesis approach enables the fast and straightforward assembly of bioactive multivalent constructs for example applicable as radiotracers for in vivo imaging with Positron Emission Tomography (PET.

  6. Study of LiBOB compound synthesis by vacuum process as lithium ion battery electrolytes

    Science.gov (United States)

    Lestariningsih, T.; Wigayati, E.; Ratri, C.; Sabrina, Q.

    2017-04-01

    Lithium bis (oxalato) borate or LiBOB is potential candidate to substitute LiPF6 which has many problems in lithium ion batteries. Many studies have been synthesized of electrolyte salt LiBOB to improve performance as electrolyte lithium ion batteries. In this paper we have studied the synthesis of compounds LiBOB undergoing pre-heat treatment in a vacuum. LiBOB was synthesized by mixing technical grade raw materials H2C2O4.2H2O, LiOH and H3BO3. The mixture H2C2O4.2H2O and LiOH was preheated at 60 °C for 2 h before adding H3BO3 in several time to be mortared in vacuum dryer, the mixture of the three starting materials was preheated in two steps at 70 °C for 6 h and the third step of preheating at a temperature of 100 °C. This powder was then characterized using XRD, FTIR and BET. The characterization results of LiBOB compared to commercial LiBOB powder. The XRD analysis results showed that the sample have formed LiBOB and LiBOB hydrate phase, while FTIR analysis results show the formation of functional groups of LiBOB. In addition, the BET results shows the surface area of synthesized LiBOB is 75.994 m2/g, close the surface area of commercial LiBOB, i.e 108.776 m2/g.

  7. 78 FR 72897 - Draft Guidance for Industry on Interim Product Reporting for Human Drug Compounding Outsourcing...

    Science.gov (United States)

    2013-12-04

    ... Human Drug Compounding Outsourcing Facilities Under Section 503B of the Federal Food, Drug, and Cosmetic... entitled ``Interim Product Reporting for Human Drug Compounding Outsourcing Facilities Under Section 503B... register as outsourcing facilities (outsourcing facilities). DATES: Although you can comment on...

  8. First coordination compounds based on a bis(imino nitroxide) biradical and 4f metal ions: synthesis, crystal structures and magnetic properties.

    Science.gov (United States)

    Reis, Samira G; Briganti, Matteo; Martins, Daniel O T A; Akpinar, Handan; Calancea, Sergiu; Guedes, Guilherme P; Soriano, Stéphane; Andruh, Marius; Cassaro, Rafael A A; Lahti, Paul M; Totti, Federico; Vaz, Maria G F

    2016-02-21

    The synthesis, crystal structures and magnetic properties of two families of heterospin complexes containing lanthanide ions and a bis(imino nitroxide) biradical (IPhIN = 1-iodo-3,5-bis(4',4',5',5'-tetramethyl-4',5'-dihydro-1H-imidazole-1'-oxyl)benzene) are reported: in [Ln2(hfac)6(IPhIN)(H2O)2] compounds, two lanthanide ions [Ln = Gd(III) (1) and Dy(III) (2)] are coordinated to the biradical, and in [Ln(hfac)3(IPhIN)(H2O)] compounds, one lanthanide ion (Ln = Tb(III) (3), Gd(III) (4) or Dy(III) (5)) is coordinated to the biradical. Ferromagnetic intramolecular magnetic interactions between Gd(III) and the biradical were found for 1 and 4, while intramolecular magnetic interactions between the radicals were ferro- and antiferromagnetic, respectively. Compound 2 shows a field induced slow relaxation of magnetization, which (under an external applied field of 2 kOe) exhibits an activation energy barrier of ΔE/kB = 27 K and a pre-exponential factor of 1.4 × 10(-8) s. To support the magnetic characterization of compound 3ab initio calculations were also performed.

  9. Degradable Polymers and Block Copolymers from Electron-deficient Carbonyl Compounds (STIR) (7.3 Polymer Chemistry - Synthesis: Architecture and Composition)

    Science.gov (United States)

    2015-04-23

    patterned surfaces and in a range of applications as surfactants and drug delivery agents. There are very few synthetic routes to polyacetals that have...deficient Carbonyl Compounds (STIR) (7.3 Polymer Chemistry - Synthesis: Architecture and Composition) The views, opinions and/or findings contained in...Degradable Polymers and Block Copolymers from Electron-deficient Carbonyl Compounds (STIR) (7.3 Polymer Chemistry - Synthesis: Architecture and

  10. Synthesis of Fuels and Value-Added Nitrogen-Containing Compounds from N2

    Science.gov (United States)

    2014-11-24

    The Haber-Bosch ammonia synthesis is one of the great technological achievements of the 20th century, having revolutionized agriculture and hence the...to ammonia synthesis , NH3 oxidation has received much less attention, and inspiration from Nature is limited as NH3 oxidations, including those...abundant metal catalysts. This fundamental scientific challenge, along with carbon neutral ammonia synthesis , has been the core of our AFOSR funded

  11. Compound Odontoma with an Unusual Appearance: Case Report

    Directory of Open Access Journals (Sweden)

    Mahdi Niknami

    2016-10-01

    Full Text Available The term odontoma is used to identify a tumor that is characterized by the production of mature enamel, dentin, cementum and pulp tissue and may interfere with the eruption of the associated tooth. The present report describes an odontoma in a 13-year-old boy, which is associated with an impacted tooth through a canal

  12. Hydrothermal synthesis of nanocubes of sillenite type compounds for photovoltaic applications and solar energy conversion of carbon dioxide to fuels

    Energy Technology Data Exchange (ETDEWEB)

    Subramanian, Vaidyanathan; Murugesan, Sankaran

    2014-04-29

    The present invention relates to formation of nanocubes of sillenite type compounds, such as bismuth titanate, i.e., Bi.sub.12TiO.sub.20, nanocubes, via a hydrothermal synthesis process, with the resulting compound(s) having multifunctional properties such as being useful in solar energy conversion, environmental remediation, and/or energy storage, for example. In one embodiment, a hydrothermal method is disclosed that transforms nanoparticles of TiO.sub.2 to bismuth titanate, i.e., Bi.sub.12TiO.sub.20, nanocubes, optionally loaded with palladium nanoparticles. The method includes reacting titanium dioxide nanotubes with a bismuth salt in an acidic bath at a temperature sufficient and for a time sufficient to form bismuth titanate crystals, which are subsequently annealed to form bismuth titanate nanocubes. After annealing, the bismuth titanate nanocubes may be optionally loaded with nano-sized metal particles, e.g., nanosized palladium particles.

  13. Diarylplatinum(II Compounds as Versatile Metallating Agents in the Synthesis of Cyclometallated Platinum Compounds with N-Donor Ligands

    Directory of Open Access Journals (Sweden)

    Margarita Crespo

    2014-03-01

    Full Text Available This review deals with the reactions of diarylplatinum(II complexes with N-donor ligands to produce a variety of cycloplatinated compounds including endo-five-, endo-seven-, endo-six- or exo-five-membered platinacycles. The observed reactions result from a series of oxidative addition/reductive elimination processes taking place at platinum(II/platinum(IV species and involving C–X (X = H, Cl, Br bond activation, arene elimination, and, in some cases, Caryl–Caryl bond formation.

  14. Metal-based ethanolamine-derived compounds: a note on their synthesis, characterization and bioactivity.

    Science.gov (United States)

    Amjad, Muhammad; Sumrra, Sajjad H; Akram, Muhammad Safwan; Chohan, Zahid H

    2016-01-01

    Metal-based ethanolamines, (L(1))-(L(4)) coordinated with Co(II), Cu(II), Ni(II) and Zn(II) metals in 1:2 (metal:ligand) molar ratio to produce new compounds have been reported. These compounds were screened for their bactericidal/fungicidal activity against a number of bacterial (Escherichia coli, Shigella flexneri, Pseudomonas aeruginosa, Salmonella typhi, Staphylococcus aureus and Bacillus subtilis) and fungal strains (Trichophyton longifusus, Candida albicans, Aspergillus flavus, Microsporum canis, Fusarium solani and Candida glabrata) alongside against a shrimp species known as Artemia salina. The screening results indicated that metal complexes have significantly higher activity than uncomplexed ligands against one or more bacterial/fungal species due to chelation. The ligand (L(4)) displayed good bacterial and fungal activity as compared to other ligands. The antibacterial results revealed that the Zn(II) complex (16) of (L(4)) was found to be the most active complex and Co(II) complex (14) of the same ligand (L(4)), demonstrated the highest antifungal activity.

  15. New 1,3,4-thiadiazole compounds including pyrazine moiety: Synthesis, structural properties and antimicrobial features

    Science.gov (United States)

    Gür, Mahmut; Şener, Nesrin; Muğlu, Halit; Çavuş, M. Serdar; Özkan, Osman Emre; Kandemirli, Fatma; Şener, İzzet

    2017-07-01

    In the study, some new 1,3,4-thiadiazole compounds were synthesized and we have reported identification of the structures by using UV-Vis, FT-IR, 1H NMR, 13C NMR and Mass spectroscopic methods. Antimicrobial activities of the compounds against three microorganisms, namely, Candida albicans ATCC 26555, Staphylococcus aureus ATCC 9144, and Escherichia coli ATCC 25922 were investigated by using disk diffusion method. These thiadiazoles exhibited an antimicrobial activity against Staphylococcus aureus and Candida albicans. The experimental data was supported by the quantum chemical calculations. Density functional theory (DFT) calculations were carried out to obtain the ground state optimized geometries of the molecules using the B3LYP, M06 and PBE1PBE methods with 3-21 g, 4-31 g, 6-311++g(2d,2p), cc-pvtz and cc-pvqz basis sets in the different combinations. Frontier molecular orbitals (FMOs) energies, band gap energies and some chemical reactivity parameters were calculated by using the aforementioned methods and basis sets, and the results were also compared with the experimental UV-Vis data.

  16. Synthesis, Structure, and Reactivity of Anionic sp(2) -sp(3) Diboron Compounds: Readily Accessible Boryl Nucleophiles.

    Science.gov (United States)

    Pietsch, Sabrina; Neeve, Emily C; Apperley, David C; Bertermann, Rüdiger; Mo, Fanyang; Qiu, Di; Cheung, Man Sing; Dang, Li; Wang, Jianbo; Radius, Udo; Lin, Zhenyang; Kleeberg, Christian; Marder, Todd B

    2015-05-04

    Lewis base adducts of tetra-alkoxy diboron compounds, in particular bis(pinacolato)diboron (B2 pin2 ), have been proposed as the active source of nucleophilic boryl species in metal-free borylation reactions. We report the isolation and detailed structural characterization (by solid-state and solution NMR spectroscopy and X-ray crystallography) of a series of anionic adducts of B2 pin2 with hard Lewis bases, such as alkoxides and fluoride. The study was extended to alternative Lewis bases, such as acetate, and other diboron reagents. The B(sp(2) )-B(sp(3) ) adducts exhibit two distinct boron environments in the solid-state and solution NMR spectra, except for [(4-tBuC6 H4 O)B2 pin2 ](-) , which shows rapid site exchange in solution. DFT calculations were performed to analyze the stability of the adducts with respect to dissociation. Stoichiometric reaction of the isolated adducts with two representative series of organic electrophiles-namely, aryl halides and diazonium salts-demonstrate the relative reactivities of the anionic diboron compounds as nucleophilic boryl anion sources.

  17. Green synthesis of some novel dioxolane compounds from Indonesian essential oils as potential biogreases

    Science.gov (United States)

    Wahyuningsih, Tutik Dwi; Kurniawan, Yehezkiel Steven

    2017-03-01

    Greases are mostly prepared from petroleum base stocks that make it toxic to the environment. The demand for green greases has led to in depth research of other renewable resources. Vegetable oils are promising candidates due to their renewability and low toxicity. However, it has poor oxidation stability and high total acid number. One way to solve this problem is chemical modification of its fatty acid structure. We report some novel dioxolane compounds from oleic acid and benzaldehyde derivates from some Indonesian essential oils via several steps, i.e: hydroxylation, esterification and acetalization. The esterification and acetalization reaction was carried out by green procedure using sonochemical method and montmorillonite KSF as a catalyst. Hydroxylation of Oleic acid was performed by KMnO4 to give 9,10-dihydroxyoctadecanoic (DHOA) in 47% yield. The esterification was done using methanol yielded methyl 9,10-dihydroxyoctadecanoate (MDHO) as white powder in 94%. Acetalization of the ester MDO with various benzaldehyde derivatives was carried out to give the dioxolan derivatives in the range of 17 - 60% yield. All of the structure was confirmed by FT-IR and GC-MS, meanwhile their physicochemical properties were determined using ASTM methods. From physicochemical properties, i.e: -TAN, TBN and IV-, it can be concluded that these novel compounds have the potential to be developed into biogrease.

  18. Synthesis of a Novel Series of S-Alkyl Thiobenzoate Compounds as Farnesyltransferase Inhibitors

    Institute of Scientific and Technical Information of China (English)

    Sheng Biao WAN; Jun FENG; Feng Ming CHU; Zong Ru GUO

    2005-01-01

    S-akyl thiobenzoate compounds were designed as famesyltransferase (FTase) inhibitors.An effective synthetic method was explored. The structures of the target compounds were elucidated by NMR spectral and elemental analysis.

  19. A new general pathway for synthesis of reference compounds of N-terminal valine-isocyanate adducts.

    Science.gov (United States)

    Davies, Ronnie; Rydberg, Per; Westberg, Emelie; Motwani, Hitesh V; Johnstone, Erik; Törnqvist, Margareta

    2010-03-15

    Adducts to Hb could be used as biomarkers to monitor exposure to isocyanates. Particularly useful is the measurement of carbamoylation of N-terminal valines in Hb, after detachment as hydantoins. The synthesis of references from the reactive isocyanates, especially diisocyanates, has been problematic due to side reactions and polymerization of the isocyanate starting material. A simpler, safer, and more general method for the synthesis of valine adducts of isocyanates has been developed using N-[(4-nitrophenyl)carbamate]valine methylamide (NPCVMA) as the key precursor to adducts of various mono- and diisocyanates of interest. By reacting NPCVMA with a range of isocyanate-related amines, carbamoylated valines are formed without the use of the reactive isocyanates. The carbamoylated products synthesized here were cyclized with good yields of the formed hydantoins. The carbamoylated derivative from phenyl isocyanate also showed quantitative yield in a test with cyclization under the conditions used in blood. This new pathway for the preparation of N-carbamoylated model compounds overcomes the above-mentioned problems in the synthesis and is a general and simplified approach, which could make such reference compounds of adducts to N-terminal valine from isocyanates accessible for biomonitoring purposes. The synthesized hydantoins corresponding to adducts from isocyanic acid, methyl isocyanate, phenyl isocyanate, and 2,6-toluene diisocyanate were characterized by LC-MS analysis. The background level of the hydantoin from isocyanic acid in human blood was analyzed with the LC-MS conditions developed.

  20. Towards new binary compounds: Synthesis of amorphous phosphorus carbide by pulsed laser deposition

    Energy Technology Data Exchange (ETDEWEB)

    Hart, Judy N., E-mail: Judy.Hart@bristol.ac.uk [School of Chemistry, University of Bristol, Bristol BS8 1TS (United Kingdom); May, Paul W.; Allan, Neil L. [School of Chemistry, University of Bristol, Bristol BS8 1TS (United Kingdom); Hallam, Keith R. [Interface Analysis Centre, University of Bristol, 121 St. Michaels Hill, Bristol BS2 8BS (United Kingdom); Claeyssens, Frederik [Kroto Research Institute, Department of Materials Science and Engineering, University of Sheffield, Broad Lane, Sheffield S3 7HQ (United Kingdom); Fuge, Gareth M.; Ruda, Michelle [School of Chemistry, University of Bristol, Bristol BS8 1TS (United Kingdom); Heard, Peter J. [Interface Analysis Centre, University of Bristol, 121 St. Michaels Hill, Bristol BS2 8BS (United Kingdom)

    2013-02-15

    We have recently undertaken comprehensive computational studies predicting possible crystal structures of the as yet unknown phosphorus carbide as a function of composition. In this work, we report the synthesis of amorphous phosphorus-carbon films by pulsed laser deposition. The local bonding environments of carbon and phosphorus in the synthesised materials have been analysed by x-ray photoelectron spectroscopy; we have found strong evidence for the formation of direct P-C bonding and hence phosphorus carbide. There is a good agreement between the bonding environments found in this phosphorus carbide material and those predicted in the computational work. In particular, the local bonding environments are consistent with those found in the {beta}-InS-like structures that we predict to be low in energy for phosphorus:carbon ratios between 0.25 and 1. Highlights: Black-Right-Pointing-Pointer We have synthesised amorphous phosphorus-carbon films by pulsed laser deposition. Black-Right-Pointing-Pointer X-ray photoelectron spectroscopy results indicate formation of direct P-C bonds and hence phosphorus carbide. Black-Right-Pointing-Pointer Local bonding environments are consistent with those in predicted structures.

  1. Design, synthesis and molecular docking studies of novel triazole antifungal compounds

    Institute of Scientific and Technical Information of China (English)

    Qiu Qin He; Ke Li; Yong Bing Cao; Huan Wen Dong; Li Hua Zhao; Chao Mei Liu; Chun Quan Sheng

    2007-01-01

    Based on the active site of Candida albicans lanosterol 14α-demethylase (CACYP51), novel triazole compounds structurally different from the current triazole drugs were designed and synthesized.In vitro antifungal activities showed that compounds 10,11,16 and 20 exhibited strong activities.In addition, compounds 10,11 and 16 also displayed certain activities against fluconazole-resistant fungi.

  2. Hexa- and dodecanuclear polyoxomolybdate cyclic compounds: application toward the facile synthesis of nanoparticles and film electrodeposition.

    Science.gov (United States)

    Dolbecq, Anne; Compain, Jean-Daniel; Mialane, Pierre; Marrot, Jérôme; Sécheresse, Francis; Keita, Bineta; Holzle, Luis Roberto Brudna; Miserque, Frédéric; Nadjo, Louis

    2009-01-01

    Two new compounds based on O(3)PCH(2)PO(3)(4-) ligands and {Mo(V)(2)O(4)} dimeric units have been synthesized and structurally characterized. The dodecanuclear Mo(V) polyoxomolybdate species in (NH(4))(18)[(Mo(V)(2)O(4))(6)(OH)(6)(O(3)PCH(2)PO(3))(6)] x 33 H(2)O (1) is a cyclohexane-like ring in a chair conformation with pseudo S(6) symmetry. In the solid state, the wheels align side by side, thus delimiting large rectangular voids. The hexanuclear anion in Na(8)[(Mo(V)(2)O(4))(3)(O(3)PCH(2)PO(3))(3)(CH(3)AsO(3))] x 19 H(2)O (2) has a triangular framework and encapsulates a methylarsenato ligand. (31)P NMR spectroscopic analysis revealed the stability of 2 in various aqueous media, whereas the stability of 1 depends on the nature of the cations present in solution. It has been evidenced that the transformation of 1 into 2 occurs in the presence of CH(3)AsO(3)(2-) ions. This behavior shows that 1 can be used as a new precursor for the synthesis of Mo(V)/diphosphonate systems. The two complexes were very efficient both as reductants of Pt and Pd metallic salts and as capping agents for the resulting Pt(0) and Pd(0) nanoparticles. The size of the obtained nanoparticles depends both on the nature of the polyoxometalate (POM; i.e., 1 or 2) and on the [metallic salt]/[POM] ratio. In all cases, X-ray photoelectron spectroscopy (XPS) measurements have revealed the presence of Mo(VI) species that stabilize the nanoparticles and the absence of Mo(V) moieties. Diffuse-reflectance FTIR spectra of the Pt nanoparticles show that the capping Mo(VI) POMs are identical for both systems and contain the diphosphonato ligand. The colloidal solutions do not show any precipitate and the nanoparticles remain well-dispersed for several months. The electrochemical reduction of Mo(V) species was studied for 2. Cyclic voltammetry alone and electrochemical quartz crystal microbalance coupled with cyclic voltammetry show the deposition of a film on the electrode surface during this reduction.

  3. Synthesis and Evaluation of a Library of Trifunctional Scaffold-Derived Compounds as Modulators of the Insulin Receptor.

    Science.gov (United States)

    Fabre, Benjamin; Pícha, Jan; Vaněk, Václav; Selicharová, Irena; Chrudinová, Martina; Collinsová, Michaela; Žáková, Lenka; Buděšínský, Miloš; Jiráček, Jiří

    2016-12-12

    We designed a combinatorial library of trifunctional scaffold-derived compounds, which were derivatized with 30 different in-house-made azides. The compounds were proposed to mimic insulin receptor (IR)-binding epitopes in the insulin molecule and bind to and activate this receptor. This work has enabled us to test our synthetic and biological methodology and to prove its robustness and reliability for the solid-phase synthesis and testing of combinatorial libraries of the trifunctional scaffold-derived compounds. Our effort resulted in the discovery of two compounds, which were able to weakly induce the autophosphorylation of IR and weakly bind to this receptor at a 0.1 mM concentration. Despite these modest biological results, which well document the well-known difficulty in modulating protein-protein interactions, this study represents a unique example of targeting the IR with a set of nonpeptide compounds that were specifically designed and synthesized for this purpose. We believe that this work can open new perspectives for the development of next-generation insulin mimetics based on the scaffold structure.

  4. Synthesis and preliminary evaluation of N-acylhydrazone compounds as antibacterial and antifungal agents; Sintese e avaliacao preliminar da atividade antibacteriana e antifungica de derivados N-acilidrazonicos

    Energy Technology Data Exchange (ETDEWEB)

    Cachiba, Thomas Haruo; Carvalho, Bruno Demartini; Carvalho, Diogo Teixeira [Universidade Federal de Alfenas, MG (Brazil). Fac. de Ciencias Farmaceuticas. Dept. de Alimentos e Medicamentos; Cusinato, Marina; Prado, Clara Gaviao; Dias, Amanda Latercia Tranches, E-mail: diogo.carvalho@unifal-mg.edu.br [Universidade Federal de Alfenas, MG (Brazil). Inst. de Ciencias Biomedicas

    2012-07-01

    We describe the synthesis and evaluation of N-acylhydrazone compounds bearing different electron-donating groups in one of its aromatic rings, obtained using a four-step synthetic route. IC{sub 50} values against pathogenic fungi and bacteria were determined by serial microdilution. Compounds showed low activity against Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa. By contrast, a derivative with a meta-oriented electron-donating group showed significant activity (IC50) against Candida albicans (17 {mu}M), C. krusei (34 {mu}M) and C. tropicalis (17 {mu}M). Results suggest this is a promising lead-compound for synthesis of potent antifungal agents. (author)

  5. Ozonolysis of unsaturated compounds in the synthesis of insect pheromones and juvenoids

    Science.gov (United States)

    Ishmuratov, Gumer Yu; Kharisov, Rinat Ya; Odinokov, Viktor N.; Tolstikov, Genrikh A.

    1995-06-01

    The review surveys data on the use of the ozonolysis of cyclic and acyclic monoenes, dienes, and trienes in various stages of the total synthesis of insect pheromones and juvenoids. The bibliography includes 178 references.

  6. The Synthesis of Imidazoline Derivative Compounds as Corrosion Inhibitor towards Carbon Steel in 1% NaCl Solution

    Directory of Open Access Journals (Sweden)

    Deana Wahyuningrum

    2008-03-01

    Full Text Available Oleic imidazoline is one of the nitrogen containing heterocyclic compounds that has been widely used as commercial corrosion inhibitor, especially in minimizing the carbon dioxide induced corrosion process in oilfield mining. In this present work, some imidazoline derivative compounds have been synthesized utilizing both conventional and microwave assisted organic synthesis (MAOS methods, in order to determine their corrosion inhibition properties on carbon steel surface. The MAOS method is more effective in synthesizing these compounds than the conventional method regarding to the higher chemical yields of products (91% to 94% and the shorter reaction times (7 to 10 minutes. The characterization of corrosion inhibition activities of the synthesized products towards carbon steel in 1% NaCl solution was determined by the Tafel plot method. The corrosion inhibition activities of compound 1b ((Z-2-(2-(heptadec-8-enyl-4,5-dihydroimidazol-1-ylethanamine, 2b ((Z-2-(2-(heptadec-8-enyl-4,5-dihydroimidazol-1-ylethanol and 3b (2-(2-heptadecyl-4,5-dihydroimidazol-1-ylethanamine at 8 ppm concentration in 1% NaCl solution are, respectively, 32.18%, 39.59% and 12.73%. The heptadec-8-enyl and hydroxyethyl substituents at C(2 and N(1 position of imidazoline ring, respectively, gave the most effective corrosion inhibition activity towards carbon steel compared to the presence of other substituents. The increase in concentrations of compound 1b, 2b and 3b in 1% NaCl solution tends to improve their corrosion inhibition activities. Based on the analysis of the free Gibbs adsorption energy (DG0ads values of compound 1b, 2b and 3b (-32.97, -34.34 and -31.27 kJ/mol, respectively, these compounds have the potential to interact with carbon steel through semi-physiosorption or semi-chemisorption.

  7. Prediction of Multi-Target Networks of Neuroprotective Compounds with Entropy Indices and Synthesis, Assay, and Theoretical Study of New Asymmetric 1,2-Rasagiline Carbamates

    Directory of Open Access Journals (Sweden)

    Francisco J. Romero Durán

    2014-09-01

    Full Text Available In a multi-target complex network, the links (Lij represent the interactions between the drug (di and the target (tj, characterized by different experimental measures (Ki, Km, IC50, etc. obtained in pharmacological assays under diverse boundary conditions (cj. In this work, we handle Shannon entropy measures for developing a model encompassing a multi-target network of neuroprotective/neurotoxic compounds reported in the CHEMBL database. The model predicts correctly >8300 experimental outcomes with Accuracy, Specificity, and Sensitivity above 80%–90% on training and external validation series. Indeed, the model can calculate different outcomes for >30 experimental measures in >400 different experimental protocolsin relation with >150 molecular and cellular targets on 11 different organisms (including human. Hereafter, we reported by the first time the synthesis, characterization, and experimental assays of a new series of chiral 1,2-rasagiline carbamate derivatives not reported in previous works. The experimental tests included: (1 assay in absence of neurotoxic agents; (2 in the presence of glutamate; and (3 in the presence of H2O2. Lastly, we used the new Assessing Links with Moving Averages (ALMA-entropy model to predict possible outcomes for the new compounds in a high number of pharmacological tests not carried out experimentally.

  8. Synthesis of the Demospongic Compounds, (6Z, 11Z-Octadecadienoic Acid and (6Z, 11Z-Eicosadienoic Acid

    Directory of Open Access Journals (Sweden)

    V. R. Mamdapur

    1997-01-01

    Full Text Available A stereoselective synthesis of (6Z, 11Z-octadecadienoic acid (1 and (6Z, 11Z-eicosadienoic acid (2 from easily accessible pentane-1,5-diol (3 is described. Thus, compound 3 on pyranylation and oxidation gave the aldehyde 5 which was converted to the acid 7 by Wittig reaction with a suitable phosphorane. Its depyranylation and oxidation furnished the key aldehyde 9 which upon Wittig reaction with n-heptylidene and n-nonylidene phosphoranes, respectively followed by alkaline hydrolysis afforded the title acids.

  9. Pathways for synthesis of new selenium-containing oxo-compounds: Chemical vapor transport reactions, hydrothermal techniques and evaporation method

    Science.gov (United States)

    Kovrugin, Vadim M.; Colmont, Marie; Siidra, Oleg I.; Gurzhiy, Vladislav V.; Krivovichev, Sergey V.; Mentré, Olivier

    2017-01-01

    Due to the low and close melting and sublimation temperatures (340 and 350 °C, respectively), the crystal growth of selenates and/or selenites is generally achieved using either chemical vapor transport routes, hydrothermal methods due to the good solubility and reactivity of (SeO3)2- anions or isothermal evaporation synthesis. Here we report examples many new crystal structures obtained using these synthesis routes. Particularly, description of each process is given with theoretical and practical information assorted with description of selected structures.

  10. Enzymes useful for chiral compound synthesis: structural biology, directed evolution, and protein engineering for industrial use.

    Science.gov (United States)

    Kataoka, Michihiko; Miyakawa, Takuya; Shimizu, Sakayu; Tanokura, Masaru

    2016-07-01

    Biocatalysts (enzymes) have many advantages as catalysts for the production of useful compounds as compared to chemical catalysts. The stereoselectivity of the enzymes is one advantage, and thus the stereoselective production of chiral compounds using enzymes is a promising approach. Importantly, industrial application of the enzymes for chiral compound production requires the discovery of a novel useful enzyme or enzyme function; furthermore, improving the enzyme properties through protein engineering and directed evolution approaches is significant. In this review, the significance of several enzymes showing stereoselectivity (quinuclidinone reductase, aminoalcohol dehydrogenase, old yellow enzyme, and threonine aldolase) in chiral compound production is described, and the improvement of these enzymes using protein engineering and directed evolution approaches for further usability is discussed. Currently, enzymes are widely used as catalysts for the production of chiral compounds; however, for further use of enzymes in chiral compound production, improvement of enzymes should be more essential, as well as discovery of novel enzymes and enzyme functions.

  11. Synthesis and biological evaluation of 4-(hydroxyalkyl)estradiols and related compounds.

    Science.gov (United States)

    Lovely, C J; Bhat, A S; Coughenour, H D; Gilbert, N E; Brueggemeier, R W

    1997-11-07

    A series of synthetic estrogens containing hydroxyalkyl side chains at the C-4 position of the A ring were designed as metabolically stable analogs of 4-hydroxyestradiol, a catechol estrogen. These synthetic steroids would facilitate investigations on the potential biological role of catechol estrogens and also enable further examination of the structural and electronic constraints on the A ring in the interaction of estrogens with the estrogen receptor. Catechol estrogens are implicated as possible causative agents in estrogen-induced tumorigenesis. 4-Hydroxyestradiol has weaker affinity for the estrogen receptor and exhibits lower estrogenic activity in vivo; on the other hand, the catechol estrogens are prone to further oxidative metabolism and can form reactive intermediates. This report describes the synthesis and initial biochemical evaluation of 4-(hydroxyalkyl)estrogens and 4-(aminoalkyl)estradiols. The 4-(hydroxyalkyl)estrogens were prepared by oxidative hydroboration of 4-alkenylestradiols. The alkenylestradiols were obtained via a Stille cross-coupling between a MOM-protected 4-bromoestradiol and an alkenylstannane. The (4-aminoalkyl)estrogens were prepared from the hydroxyalkyl derivatives with phthalimide under Mitsunobu conditions. The substituted estradiols were evaluated for estrogen receptor binding activity in MCF-7 human mammary carcinoma cells, and 4-(hydroxymethyl)estradiol 1 exhibited the highest affinity with an apparent EC50 value of 364 nM. The relative activities for mRNA induction of the pS2 gene in MCF-7 cell cultures by the 4-(hydroxyalkyl)estrogens closely parallel the relative binding affinities. 4-(Hydroxymethyl)estradiol 1 did not stimulate the growth of MCF-7 cells at concentrations up to 1 microM. Thus, 4-(hydroxymethyl)estradiol 1 exhibited similar estrogen receptor affinity as the catechol estrogen, 4-hydroxyestradiol, and may prove useful in the examination of the biological effects of 4-hydroxyestrogens.

  12. Design, synthesis and in vitro antimalarial evaluation of triazole-linked chalcone and dienone hybrid compounds.

    Science.gov (United States)

    Guantai, Eric M; Ncokazi, Kanyile; Egan, Timothy J; Gut, Jiri; Rosenthal, Philip J; Smith, Peter J; Chibale, Kelly

    2010-12-01

    A targeted series of chalcone and dienone hybrid compounds containing aminoquinoline and nucleoside templates was synthesized and evaluated for in vitro antimalarial activity. The Cu(I)-catalyzed cycloaddition of azides and terminal alkynes was applied as the hybridization strategy. Several chalcone-chloroquinoline hybrid compounds were found to be notably active, with compound 8b the most active, exhibiting submicromolar IC(50) values against the D10, Dd2 and W2 strains of Plasmodium falciparum.

  13. Synthesis and crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Delgado, Gerzon E., E-mail: gerzon@ula.ve [Laboratorio de Cristalografía, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of); Quintero, Eugenio; Tovar, Rafael; Grima-Gallardo, Pedro; Quintero, Miguel [Centro de Estudio de Semiconductores, Departamento de Física, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of)

    2014-11-15

    Highlights: • New quaternary compound. • Synthesis from solid state reaction. • Crystal structure. • Rietveld refinement. - Abstract: The crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}, belonging to the system I–II{sub 2}–III–VI{sub 4}, was characterized by Rietveld refinement using X-ray powder diffraction data. The powder pattern was composed by 84.5% of the principal phase AgFe{sub 2}GaTe{sub 4} and 15.5% of the secondary phase FeTe. This material crystallizes with stannite structure in the tetragonal space group I-42m (N° 121), Z = 2, unit cell parameters a = 6.3409(2) Å, c = 12.0233(4) Å, V = 483.42(3) Å{sup 3}, and is isostructural with CuFe{sub 2}InSe{sub 4}.

  14. Synthesis and study on biological activity of nitrogen-containing heterocyclic compounds – regulators of enzymes of nucleic acid biosynthesis

    Directory of Open Access Journals (Sweden)

    Alexeeva I. V.

    2013-07-01

    Full Text Available Results of investigations on the development of new regulators of functional activity of nucleic acid biosynthesis enzymes based on polycyclic nitrogen-containing heterosystems are summarized. Computer design and molecular docking in the catalytic site of target enzyme (T7pol allowed to perform the directed optimization of basic structures. Several series of compounds were obtained and efficient inhibitors of herpes family (simple herpes virus type 2, Epstein-Barr virus, influenza A and hepatitis C viruses were identified, as well as compounds with potent antitumor, antibacterial and antifungal activity. It was established that the use of model test systems based on enzymes participating in nucleic acids synthesis is a promising approach to the primary screening of potential inhibitors in vitro.

  15. Synthesis and Structures of [LCu(I)(SSi(i)Pr3)] (L = triphos, carbene) and Related Compounds.

    Science.gov (United States)

    Ferrara, Skylar J; Wang, Bo; Haas, Elaine; Wright LeBlanc, Karry; Mague, Joel T; Donahue, James P

    2016-09-19

    The mononuclear Cu(I) complexes [LCu(I)(SSi(i)Pr3)] (L = 1,1,1-tris(diphenylphosphinomethyl)ethane (triphos), 1,3-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene (IMes)) have been prepared by ligand displacement from [LCu(I)Cl] with (i)Pr3SiS(-). Both compounds are colorless, diamagnetic species and have been characterized structurally by X-ray crystallography. The compounds [(IMes)Cu(η(1)κ(S)-SC(O)CH3)] and [(triphos)Cu(η(1)κ(S)-SC(S)OCH3)] have been prepared in the context of synthesis aimed at [LCu(η(1)κ(S)-SCOS)] and [LCu(η(1)κ(S)-SCS2)] complexes, which are intended as synthons toward an analogue of the Mo(μ-OSCO)Cu intermediate proposed as occurring in the catalytic cycle of carbon monoxide dehydrogenase (CODH).

  16. A new synthesis of Entacapone and report on related studies

    Indian Academy of Sciences (India)

    Attimogae Shivamurthy Harisha; Suresh Parameshwar Nayak; Pavan M S; Shridhara K; Sundarraja Rao K; Rajendra K; Koteppa Pari; Sivaramkrishnan H; Guru Row T N; Kuppuswamy Nagarajan

    2015-11-01

    A new synthesis of the catechol--methyltransferase (COMT) inhibitor, entacapone (E-isomer) has been achieved under mild conditions by amine-mediated demethylation of the precursor 2-Cyano-3-(3-hydroxy-4-methoxy-5-nitrophenyl) prop-2-eneamide, wherein the methoxyl group adjacent to a nitro group gets demethylated under nucleophilic attack. Similar demethylation was achieved on ethyl 2-cyano-3-(3,4-dimethoxy-5-nitrophenyl) prop-2-enoate, 2-cyano-3-(3,4-dimethoxy-5-nitrophenyl)-N,N-diethylprop-2-enamide, ethyl 2-cyano-3-(3-hydroxy-4-methoxy-5-nitrophenyl) prop-2-enoate and ethyl 2-cyano-3-(4-methoxy-3-nitrophenyl) prop-2-enoate. The scope of demethylation has been studied. Analogues of ethyl 2-cyano-3-(3,4-dimethoxy-5-nitrophenyl) prop-2-enoate wherein a methoxyl group is not adjacent to a NO2 group are unaffected and phenolic derivatives yield the amine salts. Entacapone has been converted to salts with organic bases. The crystal structure of the isomer of entacapone (Z-isomer), a significant human metabolite of E-isomer has been established. NMR methods for deriving E and Z geometry and other similar molecules have been successfully established, mainly by studying the proton coupled 13C spectra. Preliminary studies reveal in vitro activity for some compounds against tuberculosis (TB) and dengue.

  17. Nanoscale Synthesis and Characterization Laboratory Annual Report 2007

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V

    2008-04-07

    The Nanoscale Synthesis and Characterization Laboratory's (NSCL) primary mission is to create and advance interdisciplinary research and development opportunities in nanoscience and technology. The NSCL is delivering on its mission providing Laboratory programs with scientific solutions through the use of nanoscale synthesis and characterization. While this annual report summarizes 2007 activities, we have focused on nanoporous materials, advanced high strength, nanostructured metals, novel 3-dimensional lithography and characterization at the nanoscale for the past 3 years. In these three years we have synthesized the first monolithic nanoporous metal foams with less than 10% relative density; we have produced ultrasmooth nanocrystalline diamond inertial confinement fusion capsules; we have synthesized 3-dimensional graded density structures from full density to 5% relative density using nanolithography; and we have established ultrasmall angle x-ray scattering as a non-destructive tool to determine the structure on the sub 300nm scale. The NSCL also has a mission to recruit and to train personnel for Lab programs. The NSCL continues to attract talented scientists to the Laboratory. Andrew Detor from Massachusetts Institute of Technology, Sutapa Ghosal from the University of California, Irvine, Xiang Ying Wang from Shanghai Institute of Technology, and Arne Wittstock from University of Bremen joined the NSCL this year. The NSCL is pursuing four science and technology themes: nanoporous materials, advanced nanocrystalline materials, novel three-dimensional nanofabrication technologies, and nondestructive characterization at the mesoscale. The NSCL is also pursuing building new facilities for science and technology such as nanorobotics and atomic layer deposition.

  18. Synthesis and toxicity evaluation of hydrophobic ionic liquids for volatile organic compounds biodegradation in a two-phase partitioning bioreactor

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez Castillo, Alfredo Santiago [Ecole Nationale Supérieure de Chimie de Rennes, CNRS, UMR 6226, 11 Allée de Beaulieu, CS 50837, 35708 Rennes Cedex 7 (France); Université européenne de Bretagne (France); Guihéneuf, Solène, E-mail: solene.guiheneuf@wanadoo.fr [Université européenne de Bretagne, Université de Rennes 1, Sciences Chimiques de Rennes, UMR, CNRS 6226, Groupe Ingénierie Chimique & Molécules Pour le Vivant (ICMV), Bât. 10A, Campus de Beaulieu, Avenue du Général Leclerc, CS 74205, 35042 Rennes cedex (France); Le Guével, Rémy [Plate-forme ImPACcell Structure Fédérative de Recherche BIOSIT Université de Rennes 1, Bat. 8, Campus de Villejean, 2 Avenue du Pr. Leon Bernard, CS 34317, 35043 Rennes Cedex (France); Biard, Pierre-François [Ecole Nationale Supérieure de Chimie de Rennes, CNRS, UMR 6226, 11 Allée de Beaulieu, CS 50837, 35708 Rennes Cedex 7 (France); Université européenne de Bretagne (France); and others

    2016-04-15

    Highlights: • Description of a VOC depollution system suitable with industrial processes, TPPB. • Novel association of TPPB and hydrophobic ionic liquids. • Synthesis of several hydrophobic ionic liquids designed to fit desired properties. • Toxicity evaluation of these ILs towards cells, animals and bacteria. - Abstract: Synthesis of several hydrophobic ionic liquids (ILs), which might be selected as good candidates for degradation of hydrophobic volatile organic compounds in a two-phase partitioning bioreactor (TPPB), were carried out. Several bioassays were also realized, such as toxicity evaluation on activated sludge and zebrafish, cytotoxicity, fluoride release in aqueous phase and biodegradability in order to verify their possible effects in case of discharge in the aquatic environment and/or human contact during industrial manipulation. The synthesized compounds consist of alkylimidazoliums, functionalized imidazoliums, isoqinoliniums, triazoliums, sulfoniums, pyrrolidiniums and morpholiniums and various counter-ions such as: PF{sub 6}{sup −}, NTf{sub 2}{sup −} and NfO{sup −}. Toxicity evaluation on activated sludge of each compound (5% v/v of IL) was assessed by using a glucose uptake inhibition test. Toxicity against zebrafish and cytotoxicity were evaluated by the ImPACCell platform of Rennes (France). Fluoride release in water was estimated by regular measurements using ion chromatography equipment. IL biodegradability was determined by measuring BOD{sub 28} of aqueous samples (compound concentration,1 mM). All ILs tested were not biodegradable; while some of them were toxic toward activated sludge. Isoquinolinium ILs were toxic to human cancerous cell lines. Nevertheless no toxicity was found against zebrafish Danio rerio. Only one IL released fluoride after long-time agitation.

  19. Neutral and ionic platinum compounds containing a cyclometallated chiral primary amine: synthesis, antitumor activity, DNA interaction and topoisomerase I-cathepsin B inhibition.

    Science.gov (United States)

    Albert, Joan; Bosque, Ramon; Crespo, Margarita; Granell, Jaume; López, Concepción; Martín, Raquel; González, Asensio; Jayaraman, Anusha; Quirante, Josefina; Calvis, Carme; Badía, Josefa; Baldomà, Laura; Font-Bardia, Mercè; Cascante, Marta; Messeguer, Ramon

    2015-08-14

    The synthesis and preliminary biological evaluation of neutral and cationic platinum derivatives of chiral 1-(1-naphthyl)ethylamine are reported, namely cycloplatinated neutral complexes [PtCl{(R or S)-NH(2)CH(CH(3))C(10)H(6)}(L)] [L = SOMe(2) ( 1-R or 1-S ), L = PPh(3) (2-R or 2-S), L = P(4-FC(6)H(4))(3) (3-R), L = P(CH(2))(3)N(3)(CH(2))(3) (4-R)], cycloplatinated cationic complexes [Pt{(R)-NH(2)CH(CH(3))C(10)H(6)}{L}]Cl [L = Ph(2)PCH(2)CH(2)PPh(2) (5-R), L = (C(6)F(5))(2)PCH(2)CH(2)P(C(6)F(5))(2) (6-R)] and the Pt(ii) coordination compound trans-[PtCl(2){(R)-NH(2)CH(CH(3))C(10)H(6)}(2)] (7-R). The X-ray molecular structure of 7-R is reported. The cytotoxic activity against a panel of human adenocarcinoma cell lines (A-549 lung, MDA-MB-231 and MCF-7 breast, and HCT-116 colon), cell cycle arrest and apoptosis, DNA interaction, topoisomerase I and cathepsin B inhibition, and Pt cell uptake of the studied compounds are presented. Remarkable cytotoxicity was observed for most of the synthesized Pt(ii) compounds regardless of (i) the absolute configuration R or S, and (ii) the coordinated/cyclometallated (neutral or cationic) nature of the complexes. The most potent compound 2-R (IC(50) = 270 nM) showed a 148-fold increase in potency with regard to cisplatin in HCT-116 colon cancer cells. Preliminary biological results point out to different biomolecular targets for the investigated compounds. Neutral cyclometallated complexes 1-R and 2-R, modify the DNA migration as cisplatin, cationic platinacycle 5-R was able to inhibit topoisomerase I-promoted DNA supercoiling, and Pt(ii) coordination compound 7-R turned out to be the most potent inhibitor of cathepsin B. Induction of G-1 phase ( 2-R and 5-R ), and S and G-2 phases (6-R) arrests are related to the antiproliferative activity of some representative compounds upon A-549 cells. Induction of apoptosis is also observed for 2-R and 6-R.

  20. Synthesis, crystal structure and antibacterial activity of new highly functionalized ionic compounds based on the imidazole nucleus.

    Science.gov (United States)

    Bahnous, Mebarek; Bouraiou, Abdelmalek; Chelghoum, Meryem; Bouacida, Sofiane; Roisnel, Thierry; Smati, Farida; Bentchouala, Chafia; Gros, Philippe C; Belfaitah, Ali

    2013-03-01

    Several new highly functionalized imidazolium derivatives were synthesized, via appropriate synthetic routes, using imidazole, 1-methylimidazole and 2-phenyl-1-methylimidazole as key intermediates. The antibacterial activity of the prepared compounds was evaluated against: Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa and Salmonella thipymurium using disk-diffusion and MIC methods. Crystal X-ray structures are reported for six compounds. Copyright © 2013 Elsevier Ltd. All rights reserved.

  1. Synthesis and toxicity evaluation of hydrophobic ionic liquids for volatile organic compounds biodegradation in a two-phase partitioning bioreactor.

    Science.gov (United States)

    Rodriguez Castillo, Alfredo Santiago; Guihéneuf, Solène; Le Guével, Rémy; Biard, Pierre-François; Paquin, Ludovic; Amrane, Abdeltif; Couvert, Annabelle

    2016-04-15

    Synthesis of several hydrophobic ionic liquids (ILs), which might be selected as good candidates for degradation of hydrophobic volatile organic compounds in a two-phase partitioning bioreactor (TPPB), were carried out. Several bioassays were also realized, such as toxicity evaluation on activated sludge and zebrafish, cytotoxicity, fluoride release in aqueous phase and biodegradability in order to verify their possible effects in case of discharge in the aquatic environment and/or human contact during industrial manipulation. The synthesized compounds consist of alkylimidazoliums, functionalized imidazoliums, isoqinoliniums, triazoliums, sulfoniums, pyrrolidiniums and morpholiniums and various counter-ions such as: PF6(-), NTf2(-) and NfO(-). Toxicity evaluation on activated sludge of each compound (5% v/v of IL) was assessed by using a glucose uptake inhibition test. Toxicity against zebrafish and cytotoxicity were evaluated by the ImPACCell platform of Rennes (France). Fluoride release in water was estimated by regular measurements using ion chromatography equipment. IL biodegradability was determined by measuring BOD28 of aqueous samples (compound concentration,1mM). All ILs tested were not biodegradable; while some of them were toxic toward activated sludge. Isoquinolinium ILs were toxic to human cancerous cell lines. Nevertheless no toxicity was found against zebrafish Danio rerio. Only one IL released fluoride after long-time agitation. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Synthesis of Tetra-Schiff Base Macrocyclic Compound Containing Benzo-12-crown-4

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Tetra-Schiff base macrocyclic compound containing benzo-12-crown-4 was synthesized via condensation of 2, 6-diformyl-4-methyl-phenol with 4(, 5(- diaminobenzo-12-C- 4 promoted by proton. The compound was characterized by MS, IR 1HNMR spectroscopy and elemental analysis.

  3. Studies on Synthesis and Biological Activities of Novel Triazole compounds Containing Thiophene Groups

    Institute of Scientific and Technical Information of China (English)

    XU Liang-zhong; ZHANG Shu-sheng; HU Zhi-qiang; JIAO Kui

    2003-01-01

    Fifteen new triazole compounds containing thiophene groups were synthesized and their structures were confirmed by means of 1H NMR, IR, MS spectroscopies and elemental analyses. The preliminary biological tests show that the titled compounds exhibit some activities of fungicides and plant growth regulators.

  4. Fe-Catalyzed Olefin Hydroamination with Diazo Compounds for Hydrazone Synthesis.

    Science.gov (United States)

    Zheng, Jing; Qi, Jifeng; Cui, Sunliang

    2016-01-01

    A novel Fe-catalyzed olefin hydroamination with diazo compounds for accessing hydrazones has been developed. Diazo compounds are used as radical acceptors and can be trapped by the in situ generated alkyl radical toward C-N bond formation. The reaction conditions are mild, and the substrate scope is broad. Additionally, this hydroamination protocol is applicable for intramolecular reactions to construct diverse heterocycles.

  5. SYNTHESIS OF NOVEL FLUOROQUINOLONE-TRIAZOLE HYBRID COMPOUNDS AS ANTIMICROBIAL AGENTS

    Directory of Open Access Journals (Sweden)

    Serap Başoğlu Özdemir

    2016-10-01

    Full Text Available Abstract: The hydrazide compound (2 was synthesized starting from 1-(2-fluorophenylpiperazine via two stage. The reaction of compound (2 with different alkyl(arylisothiocyanates afforded the corresponding compounds (3a-c. 1,3-Thiazolidine derivatives (4a-c were synthesized from the treatment of (3a-c with ethyl bromoacetate. Mannich bases (6a-d were yielded the treayment of (5a-c with various suitable amines in the exictence of formaldehyde. Compound (3 derivatives were converted to 1,2,4-triazole as the starting material of fluoroquinolone analogues (11a-c. Finally synthesized compounds were examined their biological properties and some of these showed potent activity.

  6. Synthesis and Properties of Novel Aromatic Azo Compounds from Hydroxyazobenzene and Cyanuric Chloride

    Institute of Scientific and Technical Information of China (English)

    李巍巍; 徐冬梅; 张志兰; 徐颖

    2012-01-01

    A new series of aromatic azo compounds with one, two, three and five azobenzene units were facilely constructed by dehydrochlorination reaction between p-hydroxyazobenzene, 4,4'-dihydroxyazobenzene and cyanuric chloride under very mild conditions. Their solubility, crystallinity, thermostability, UV-vis absorption properties and photoisomerization behaviors were carefully examined. When the number of azobenzene unit grew, the solubility of the synthesized compounds basically decreased, the crystallinity of the synthesized compounds firstly rose then dropped, while the thermostability and UV-vis absorption ability of the synthesized compounds greatly im- proved. All the aromatic azo compounds exhibited typical reversible photoisomerization behaviors and were expected to be applied in photosensitive material areas.

  7. Synthesis by two methods and crystal structure determination of a new pyrochlore-related compound Sm{sub 2}FeTaO{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Martinez, Leticia M., E-mail: lettorresg@yahoo.com [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Ruiz-Gomez, Miguel A. [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); Figueroa-Torres, M.Z.; Juarez-Ramirez, Isaias [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Moctezuma, Edgar [Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); and others

    2012-04-16

    Graphical abstract: The monoclinic (space group C2/c) structure of a new compound, Sm{sub 2}FeTaO{sub 7} shows an alternating Sm-O and Fe/Ta-O layers. In the Fe/Ta-O layer, Fe/Ta1 and Fe/Ta3 cations are coordinated by six oxygen atoms, forming irregular octahedral interconnected into a hexagonal tungsten bronze (HTB) type network. The HTB layer is a fundamental framework in the pyrohlore-related structure. Highlights: Black-Right-Pointing-Pointer Pyrochlore-related compound Sm{sub 2}FeTaO{sub 7} prepared by solid state reaction and sol-gel. Black-Right-Pointing-Pointer Sm{sub 2}FeTaO{sub 7} crystallizes with a monoclinic crystal structure and space group C2/c. Black-Right-Pointing-Pointer The compound is synthesized by sol-gel at lower temperature and time than solid state. Black-Right-Pointing-Pointer Surface area of sol-gel Sm{sub 2}FeTaO{sub 7} is 10 times higher than that prepared by solid state. - Abstract: This paper reports on the synthesis of a new pyrochlore-related compound Sm{sub 2}FeTaO{sub 7} by both solid state reaction and sol-gel synthesis routes. Structural features were determined by X-ray powder diffraction and Rietveld refinement and were corroborated using Transmission Electron Microscopy (TEM). The results revealed that Sm{sub 2}FeTaO{sub 7} crystallized in the monoclinic system with space group C2/c and the following cell parameters: a = 13.1307(5) Angstrom-Sign , b = 7.5854(3) Angstrom-Sign , c = 11.6425(4) Angstrom-Sign and {beta} = 100.971(2) Degree-Sign . The monoclinic structure of Sm{sub 2}FeTaO{sub 7} showed an arrangement of alternating Sm-O and Fe/Ta-O layers and two types of irregular octahedra of Fe/Ta-O, which are interconnected into a hexagonal tungsten bronze (HTB)-type network. On the other hand, Sm{sub 2}FeTaO{sub 7} prepared by sol-gel was obtained with lower particle sizes than the solid state produced compound. The difference in particle size causes a difference of one order of magnitude in the specific surface area. In

  8. Novel Microwave-Assisted Synthesis of the Immunomodulator Organotellurium Compound Ammonium Trichloro(dioxoethylene-O,O'tellurate (AS101

    Directory of Open Access Journals (Sweden)

    M. Pilar Vázquez-Tato

    2014-02-01

    Full Text Available Ammonium trichloro[1,2-ethanediolato-O,O']-tellurate (AS101 is the most important synthetic Te compound from the standpoint of its biological activity. It is a potent immunomodulator with a variety of potential therapeutic applications and antitumoral action in several preclinical and clinical studies. An experimental design has been used to develop and optimize a novel microwave-assisted synthesis (MAOS of the AS101. In comparison to the results observed in the literature, refluxing Te(IV chloride and ethylene glycol in acetonitrile (Method A, or by refluxing Te(IV chloride and ammonium chloride in ethylene glycol (Method B, it was found that the developed methods in the present work are an effective alternative, because although performance slightly decreases compared to conventional procedures (75% vs. 79% by Method A, and 45% vs. 51% by Method B, reaction times decreased from 4 h to 30 min and from 4 h to 10 min, by Methods A and B respectively. MAOS is proving to be of value in the rapid synthesis of compounds with new and improved biological activities, specially based on the benefit of its shorter reaction times.

  9. PGVL Hub: An integrated desktop tool for medicinal chemists to streamline design and synthesis of chemical libraries and singleton compounds.

    Science.gov (United States)

    Peng, Zhengwei; Yang, Bo; Mattaparti, Sarathy; Shulok, Thom; Thacher, Thomas; Kong, James; Kostrowicki, Jaroslav; Hu, Qiyue; Na, James; Zhou, Joe Zhongxiang; Klatte, David; Chao, Bo; Ito, Shogo; Clark, John; Sciammetta, Nunzio; Coner, Bob; Waller, Chris; Kuki, Atsuo

    2011-01-01

    PGVL Hub is an integrated molecular design desktop tool that has been developed and globally deployed throughout Pfizer discovery research units to streamline the design and synthesis of combinatorial libraries and singleton compounds. This tool supports various workflows for design of singletons, combinatorial libraries, and Markush exemplification. It also leverages the proprietary PGVL virtual space (which contains 10(14) molecules spanned by experimentally derived synthesis protocols and suitable reactants) for lead idea generation, lead hopping, and library design. There had been an intense focus on ease of use, good performance and robustness, and synergy with existing desktop tools such as ISIS/Draw and SpotFire. In this chapter we describe the three-tier enterprise software architecture, key data structures that enable a wide variety of design scenarios and workflows, major technical challenges encountered and solved, and lessons learned during its development and deployment throughout its production cycles. In addition, PGVL Hub represents an extendable and enabling platform to support future innovations in library and singleton compound design while being a proven channel to deliver those innovations to medicinal chemists on a global scale.

  10. Solid-state synthesis of monazite-type compounds LnPO{sub 4} (Ln = La to Gd)

    Energy Technology Data Exchange (ETDEWEB)

    Bregiroux, D.; Audubert, F. [CEA Cadarache (DEN/DEC/SPUA/LTEC), 13 - Saint-Paul-lez-Durance (France). Dept. d' Etudes des Combustibles; Bregiroux, D. [Laboratoire Science des Procedes Ceramiques et de Traitements de Surface, UMR CNRS-Universite 6638, 87 - Limoges (France); Charpentier, Th.; Sakellariou, D. [CEA Saclay (DSM/DRECAM/SCM/LSDRM), CEA-CNRS URA 331, 91 - Gif-sur-Yvette (France). Direction des Sciences de la Matiere; Bernache-Assollant, D. [Ecole Nationale Superieure des Mines, CIS, 42 - Saint Etienne (France)

    2007-07-01

    This work is devoted to the synthesis of monazite-type compounds LnPO{sub 4} (with Ln = La, Ce, Pr, Nd, Sm, Eu and Gd) by solid-solid reaction between a lanthanide oxide and a phosphate precursor NH{sub 4}H{sub 2}PO{sub 4}. Starting mixtures and resulting powders were characterized by coupling different techniques, in particular thermal analysis, X-ray diffraction and MAS {sup 31}P NMR. Results are presented according to the valence state of the lanthanide element in its oxide form. The intermediate chemical reactions occurring during the firing of starting reagents are described for the first time in the case of monazite with one or several cations. It has been highlighted that the solid-state route is an efficient way in order to obtain very pure and very well crystallized monazite powder. Optimum synthesis conditions are 1350 C-2h. The synthesis of monazite powders containing several lanthanides appears to be more difficult, because all the lanthanides do not react at the same temperature, leading to the formation of heterogeneous powders. (authors)

  11. Communic Acids: Occurrence, Properties and Use as Chirons for the Synthesis of Bioactive Compounds

    Directory of Open Access Journals (Sweden)

    Alejandro F. Arteaga

    2012-02-01

    Full Text Available Communic acids are diterpenes with labdane skeletons found in many plant species, mainly conifers, predominating in the genus Juniperus (fam. Cupresaceae. In this review we briefly describe their distribution and different biological activities (anti- bacterial, antitumoral, hypolipidemic, relaxing smooth muscle, etc.. This paper also includes a detailed explanation of their use as chiral building blocks for the synthesis of bioactive natural products. Among other uses, communic acids have proven useful as chirons for the synthesis of quassinoids (formal, abietane antioxidants, ambrox and other perfume fixatives, podolactone herbicides, etc., featuring shorter and more efficient processes.

  12. A Versatile Organocatalytic Approach for the Synthesis of Enantioenriched gem-Difluorinated Compounds.

    Science.gov (United States)

    Saulnier, Steve; Ciardi, Moira; Lopez-Carrillo, Veronica; Gualandi, Andrea; Cozzi, Pier Giorgio

    2015-09-21

    The combination of a practical and highly enantioselective organocatalytic reaction, which allows the stereoselective introduction of a benzodithiol group, with a fluorination step, gives a new and effective strategy for the stereoselective synthesis of difluorinated building blocks. The benzodithiol group is a versatile and chameleonic group that can be further functionalized before fluorination, giving customized and tailored useful synthetic strategies. As an example of the application of this facile strategy, the effective enantioselective synthesis of difluoroarundic acid is described. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. THE EFFECT OF A NEW SALICYLIC ACID SYNTHESIS COMPOUNDS ADMINISTRATION ON SERUM TRANSAMINASIS

    Directory of Open Access Journals (Sweden)

    STANA LETIŢIA

    2007-01-01

    Full Text Available The chemical synthesis product is the amide of chlorine salicylic acid andsulphanilamide (5ClSA-SA. This research had as objective the effect of this productfrom salicylic acid class as a potential medicine on the serum transaminasis activity.5ClSA-SA has been administrated intraperitoneal to Wistar rats for 7 daysconsecutively determining ALT and AST transaminasis activities after 5 and 7 days.Serum transaminases had high values compared to the control sample (220% ASTand 237% ALT.This synthesis product can lead to stress that induces increasing of plasmaticenzymes activity, transaminasis being one of those.

  14. Synthesis, characterization, investigation of biological activity and theoretical studies of hydrazone compounds containing choloroacetyl group

    Science.gov (United States)

    Cukurovali, Alaaddin; Yilmaz, Engin

    2014-10-01

    In this study, three new hydrazide-hydrazone derivative compounds which contain choloroacetyl group have been synthesized and characterized. In the characterization, spectral techniques such as IR, 1H NMR, 13C NMR and UV-Vis spectroscopy techniques were used. Antibacterial effects of the synthesized compounds were investigated against Staphylococcus aureus ATCC 29213, Enterococcus faecalis ATCC 29212, Escherichia coli ATCC 25922 and Pseudomonas aeruginosa ATCC 27853. In the theoretical calculations Gaussian 09 software was used with the DFT/6-311+(d,p) basis set. Experimental X-ray analysis of compounds has not been studied. Theoretical bond lengths of synthesized compounds were compared with experimental bond lengths of a similar compound. Theoretical and experimental bond lengths are in good agreement with R2: 0.896, 0.899 and 0.900 for compounds 1, 2, and 3, respectively. For antibacterial activity, the most effective one was found to be N‧-(4-bromobenzylidene)-2-chloro-N-(4-(3-methyl-3-phenylcyclobutyl)-thiazol-2-yl) acetohydrazide against P.aeroginaosa ATTC 27853, among the studied compounds.

  15. Synthesis and characterization of montmorillonite clay intercalated with molecular magnetic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Martins, Marcel G.; Martins, Daniel O.T.A.; Carvalho, Beatriz L.C. de [Instituto de Química, Universidade Federal Fluminense, Niterói, RJ 24.020–150 (Brazil); Mercante, Luiza A. [Laboratório Nacional de Nanotecnologia para o Agronegócio (LNNA), Embrapa Instrumentação, São Carlos, SP 13560 970 (Brazil); Soriano, Stéphane [Instituto de Física, Universidade Federal Fluminense, Niterói, RJ 24.210 346 (Brazil); Andruh, Marius [Inorganic Chemistry Laboratory, Faculty of Chemistry, University of Bucharest, Str. Dumbrava Rosie nr. 23, Bucharest (Romania); Vieira, Méri D., E-mail: gqimeri@vm.uff.br [Instituto de Química, Universidade Federal Fluminense, Niterói, RJ 24.020–150 (Brazil); Vaz, Maria G.F., E-mail: mariavaz@vm.uff.br [Instituto de Química, Universidade Federal Fluminense, Niterói, RJ 24.020–150 (Brazil)

    2015-08-15

    In this work montmorillonite (MMT) clay, whose matrix was modified with an ammonium salt (hexadecyltrimethylammonium bromide – CTAB), was employed as an inorganic host for the intercalation of three different molecular magnetic compounds through ion exchange: a nitronyl nitroxide derivative 2-[4-(N-ethyl)-pyridinium]-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide (p-EtRad{sup +}) and two binuclear coordination compounds, [Ni(valpn)Ln]{sup 3+}, where H{sub 2}valpn stands for 1,3-propanediyl-bis(2-iminomethylene-6-methoxy-phenol), and Ln=Gd{sup III}; Dy{sup III}. The pristine MMT and the intercalated materials were characterized by X-ray powder diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and magnetic measurements. The X-ray diffraction data analysis showed an increase of the interlamellar space of the intercalated MMT, indicating the intercalation of the magnetic compounds. Furthermore, the magnetic properties of the hybrid compounds were investigated, showing similar behavior as the pure magnetic guest species. - Graphical abstract: Montmorillonite clay was employed as inorganic host for the intercalation of three different molecular magnetic compounds through ion exchange - Highlights: • Montmorillonite was employed as a host material. • Three molecular magnetic compounds were intercalated through ion exchange. • The compounds were successful intercalated maintaining the layered structure. • The hybrid materials exhibited similar magnetic behavior as the pure magnetic guest.

  16. Synthesis and Structural Studies of Calcium and Magnesium Phosphinate and Phosphonate Compounds

    Science.gov (United States)

    Bampoh, Victoria Naa Kwale

    The work presented herein describes synthetic methodologies leading to the design of a wide array of magnesium and calcium based phosphinate and phosphonates with possible applications as bone scaffolding materials or additives to bone cements. The challenge to the chemistry of the alkaline earth phosphonate target compounds includes poor solubility of compounds, and poorly understood details on the control of the metal's coordination environment. Hence, less is known on phosphonate based alkaline earth metal organic frameworks as compared to transition metal phosphonates. Factors governing the challenges in obtaining crystalline, well-defined magnesium and calcium solids lie in the large metal diameters, the absence of energetically available d-orbitals to direct metal geometry, as well as the overall weakness of the metal-ligand bonds. A significant part of this project was concerned with the development of suitable reaction conditions to obtain X-ray quality crystals of the reaction products to allow for structural elucidation of the novel compounds. Various methodologies to aid in crystal growth including hydrothermal methods and gel crystallization were employed. We have used phosphinate and phosphonate ligands with different number of phosphorus oxygen atoms as well as diphosphonates with different linker lengths to determine their effects on the overall structural features. An interesting correlation is observed between the dimensionality of products and the increasing number of donor oxygen atoms in the ligands as we progress from phosphinic acid to the phosphorous acids. As an example, monophosphinate ligand only yielded one-dimensional compounds, whereas the phosphonates crystallize as one and two-dimensional compounds, and the di- and triphosphonate based compounds display two or three-dimensional geometries. This thesis provides a selection of calcium and magnesium compounds with one-dimensional geometry, as represented in a calcium phosphinate to novel

  17. Synthesis and Application for polarization Optical Storage of a New Photochromic compound

    Energy Technology Data Exchange (ETDEWEB)

    Cui Shiqiang; Pu Shouzhi; Liu Weijun; Liu Gang, E-mail: pushouzhi@tsinghua.org.cn [Jiangxi Key Lab of Organic Chemistry, Jiangxi Science and Technology Normal University, Nanchang 330013 (China)

    2011-02-01

    A new photochromic compound 1-[2-methyl-5-(4-methyl-phenyl)-3-thienyl]-2-[2-methyl-5- (4-fluor-phenyl)-3-thienyl]perfluoroyclopentene (1a) was synthesized, its photochromic properties were examined, the result indicated that the color of the compound 1a changed from colorless to a blue one upon irradiation with 297 nm UV light, a new absorption maxima were observed at 577 and 581 nm in hexane and PMMA film, respectively. This new photochromic compound also exhibited remarkable optical storage character.

  18. Synthesis and Structure Characterization of Novel Triazole Compounds Containing 1,3-Dioxolane

    Institute of Scientific and Technical Information of China (English)

    XU Liang-zhong; JIAN Fang-fang; NIU Shu-yan; JIANG Zhi-guo

    2004-01-01

    Five novel triazole compounds containing group 1,3-dioxolane were designed and synthesized by taking difenoconazole as the start compound and changing diphenyl ether for benzyl phenyl ether. Their structures were confirmed by elemental analyses, 1H NMR and IR spectra. The single crystal structure of 2-[4-(2,4-dichlorophenylmethoxy]phenyl-2- (1,2,4-triazol-1-yl) methane-1, 3-dioxolane was determined by means of X-ray diffraction. The preliminary bioassays showed that the synthesized compounds exhibited some activities of fungicides and plant growth regulators.

  19. Synthesis and biological evaluation of glyco-GA compounds as anticancer agents

    Institute of Scientific and Technical Information of China (English)

    Li Qin He; Zhong Hu; La Mei Yuan; Xiao Shan Wang; Yi Hua Zhang

    2012-01-01

    A series of novel glyco-gambogic acid (GA) compounds were synthesized and evaluated for their in vitro anti-proliferative activity against human hepatocellular carcinoma (HCC) cells.All compounds showed much better aqueous solubility (0.92-1.89 mg/mL) than GA (0.013 mg/mL),and displayed potent inhibition on HCC cells (IC50:0.21-12.23 μmol/L) and little affects on non-tumor liver cells (IC50:42.56-86.43 μmol/L),suggesting that glyco-GA compounds selectively inhibit HCC proliferation,and may be promising candidates for further intensive study.

  20. Synthesis and characterization of chromogenic fluoran compounds containing 4-ketoquinazolinone moieties

    Directory of Open Access Journals (Sweden)

    RANJAN G. PATEL

    2004-05-01

    Full Text Available Chromogenic fluoran compounds containing 4-ketoquinazolinone were synthesized by reacting 2-(4-diethylamino-2-hydroxybenzoylbenzoic acid with various substituted 4-ketoquinazolinones in the presence of sulfuric acid. The 4-ketoquinazolinones were obtained by reacting various substituted benzoxazin-4-ones with 4-aminophenol or 2-nitro-p-anisidine. All the synthesized derivatives were identified by conventional methods, such as melting points, elemental analysis, IR, 1H-NMR, and UV-visible spectroscopy in organic solvent and 95 % acetic acid. All the fluoran compounds develop colour on contact with acidic or electron-accepting compounds.

  1. Tandem Mannich/Diels–Alder reactions for the synthesis of indole compound libraries

    DEFF Research Database (Denmark)

    Wu, Peng; Petersen, Michael Åxman; Petersen, Rico;

    2016-01-01

    A tandem Mannich/Diels–Alder sequence for the synthesis of small-molecule libraries with an indolyl-octahydro-3a,6-epoxy-isoindole core structure is demonstrated in this study. Representative diversification examples based on this scaffold were performed, and a library is being produced within th...

  2. Synthesis and evaluation of boron compounds for neutron capture therapy of malignant brain tumors

    Energy Technology Data Exchange (ETDEWEB)

    Soloway, A.H.

    1991-01-01

    Current progress on this research includes the synthesis of chemical structures for malignant brain tumors. These structures include boron-containing derivatives of lipophilic anticonvulsants and CNS depressants; carboranyl precursors of nucleic acids and related structures; and carboranyl amino acids. Cellular uptake and persistence studies have also been carried out with F98 rat glioma cells. 1 fig., 1 tab.

  3. Synthesis and evaluation of boron compounds for neutron capture therapy of malignant brain tumors

    Energy Technology Data Exchange (ETDEWEB)

    Soloway, A.H.; Barth, R.F.

    1990-01-01

    Boron neutron capture therapy offers the potentiality for treating brain tumors currently resistant to treatment. The success of this form of therapy is directly dependent upon the delivery of sufficient numbers of thermal-neutrons to tumor cells which possess high concentrations of B-10. The objective of this project is to develop chemical methodology to synthesize boron-containing compounds with the potential for becoming incorporated into rapidly-dividing malignant brain tumor cells and excluded from normal components of the brain and surrounding tissues, to develope biological methods for assessing the potential of the compound by use of cell culture or intratumoral injection, to develop analytical methodology for measuring boron in cells and tissue using direct current plasma atomic emission spectroscopy (DCP-AES) and alpha track autoradiography, to develop biochemical and HPLC procedures for evaluating compound uptake and tissue half-life, and to develop procedures required to assess both in vitro and vivo efficacy of BNCT with selected compounds.

  4. Synthesis and biological activity of some heterocyclic compounds containing benzimidazole and beta-lactam moiety

    Indian Academy of Sciences (India)

    K F Ansari; C Lal

    2009-11-01

    A number of 1-substituted-2-methyl benzimidazole derivatives have been synthesized and tested for their antibacterial activities. The chemical structures of the newly synthesized compounds were verified on the basis of spectral and elemental methods of analyses. Investigation of antimicrobial activity of the compounds was done by disc diffusion method using Gram-positive (S. aureus, S. mutans and B. subtilis), Gram-negative (E. coli, S. typhi and P. aeruginosa) bacteria and fungi (C. albicans, A. flavus and A. niger). Among the compounds tested 5a, 5b, 5d, 5i, 5j and 5k exhibited good antibacterial activities against Gram positive bacteria, while 5d and 5i also showed notable antifungal activity. Specially compounds 5a and 5b exhibited appreciable activity against S. aureus and B. subtilis comparable to reference drugs.

  5. Claisen, Cope and Related Rearrangements in the Synthesis of Flavour and Fragrance Compounds

    Directory of Open Access Journals (Sweden)

    Janusz Nowicki

    2000-08-01

    Full Text Available A review of the use of the Claisen, Cope and related [3,3]-sigmatropic rearrangements, sequential ("tandem" sigmatropic rearrangements and the "ene" reaction in the syntheses of flavour and fragrance compounds is presented.

  6. Organophosphorus Compound DEPBT as a Coupling Reagent for Oligopeptides and Peptoids Synthesis: Studies on Its Mechanism

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Some oligopeptidcs and peptoids were synthesized by applying the organophosphorus compound DEPBT as a coupling rcagent. D-Biotin-OOBt was obtained unexpcctcdly. A proposed reaction mechanism for DEPBT-mediated coupling was proved.

  7. Synthesis, structural and electrochemical characterization of benzimidazole compounds exhibiting a smectic C liquid crystal phase

    Science.gov (United States)

    Wei, Bingzhuo; Tan, Shuai; Liang, Ting; Cao, Siyu; Wu, Yong

    2017-04-01

    Mesomorphic benzimidazole compounds were prepared from a biphenyl benzoate based precursor by substitution reaction of alkyl bromide with 2-mercaptobenzimidazole. Molecular structures of the benzimidazole compounds were characterized by nuclear magnetic resonance (NMR), Fourier transform infrared (FT-IR) spectroscopy and elemental analysis. Differential scanning calorimetry (DSC) measurements and polarizing optical microscopic (POM) observations revealed that the benzimidazole compounds exhibited a thermotropic smectic C (SC) phase. Temperature dependent X-ray diffraction (XRD) patterns suggested a tilted bilayer smectic structure in which intermolecular hydrogen bonds between benzimidazole moieties formed lamellar arrangement. Electrochemical impedance spectroscopy (EIS) characterization suggested that the SC phase favored anhydrous proton conduction of the benzimidazole compounds and the proton conductivities showed an Arrhenius temperature dependence.

  8. Dicarboxylic esters: Useful tools for the biocatalyzed synthesis of hybrid compounds and polymers

    OpenAIRE

    Ivan Bassanini; Karl Hult; Sergio Riva

    2015-01-01

    Dicarboxylic acids and their derivatives (esters and anhydrides) have been used as acylating agents in lipase-catalyzed reactions in organic solvents. The synthetic outcomes have been dimeric or hybrid derivatives of bioactive natural compounds as well as functionalized polyesters.

  9. Compounds of lanthanide picrates and 2-azacyclononanone (aza): synthesis, characterization and thermal study

    Energy Technology Data Exchange (ETDEWEB)

    Marinho, E.P.; Araujo Melo, D.M.; Zinner, L.B.; Zinner, K. [UFRN, Natal (Brazil). Dept. de Quimica; Xavier de Matos, J.E. [Departamento de Quimica Organica e Inorganica, UFC, Caixa Postal 12200, CEP 60001-970 Fortaleza CE (Brazil)

    1998-07-24

    Addition compounds between lanthanide(III) picrates and azacyclononanone(aza) were characterized by spectroscopic, microanalytical and X-ray data, with special emphasis on thermogravimetric techniques. (orig.) 10 refs.

  10. Synthesis and Antimicrobial Activity of New Schiff Base Compounds Containing 2-Hydroxy-4-pentadecylbenzaldehyde Moiety

    Directory of Open Access Journals (Sweden)

    Gadada Naganagowda

    2014-01-01

    Full Text Available Various novel Schiff base compounds have been synthesized by reaction of 2-hydroxy-4-pentadecylbenzaldehyde with substituted benzothiophene-2-carboxylic acid hydrazide and different substituted aromatic or heterocyclic amines in the presence of acetic acid in ethanol. The structures of all these compounds were confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR, and mass spectral data and have been screened for antibacterial and antifungal activity.

  11. Characterization of rhenium compounds obtained by electrochemical synthesis after aging process

    Energy Technology Data Exchange (ETDEWEB)

    Vargas-Uscategui, Alejandro, E-mail: avargasuscat@ing.uchile.cl [Departamento de Ingeniería de Minas, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile); Mosquera, Edgar [Laboratorio de Materiales a Nanoescala, Departamento de Ciencia de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile); López-Encarnación, Juan M. [Department of Mathematics-Physics and Department of Chemistry, University of Puerto Rico at Cayey, 205 Ave. Antonio R. Barceló, Cayey, PR 00736, USA. (Puerto Rico); Chornik, Boris [Departamento de Física, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Blanco Encalada Av. 2008, Santiago (Chile); Katiyar, Ram S. [Department of Physics and Institute for Functional Nanomaterials, University of Puerto Rico San Juan, San Juan, PR 00931-3343 (United States); Cifuentes, Luis [Departamento de Ingeniería de Minas, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Tupper Av. 2069, Santiago (Chile)

    2014-12-15

    The proper identification of the molecular nature of the aged rhenium compound obtained by means of electrodeposition from an alkaline aqueous electrolyte was determined. Chemical, structural and vibrational experimental characterization of the aged Re compound showed agreement with quantum-computations, thereby allowing the unambiguous identification of the Re compound as H(ReO{sub 4})H{sub 2}O. - Graphical abstract: Rhenium oxides were electrodeposited on a copper surface and after environmental aging was formed the H(ReO{sub 4})H{sub 2}O compound. The characterization of the synthesized material was made through the comparison of experimental evidence with quantum mechanical computations carried out by means of density functional theory (DFT). - Highlights: • Aged rhenium compound obtained by means of electrodeposition was studied. • The study was made by combining experimental and DFT-computational information. • The aged electrodeposited material is consistent with the H(ReO{sub 4})H{sub 2}O compound.

  12. Exploration of Cyanine Compounds as Selective Inhibitors of Protein Arginine Methyltransferases: Synthesis and Biological Evaluation

    Science.gov (United States)

    2016-01-01

    Protein arginine methyltransferase 1 (PRMT1) is involved in many biological activities, such as gene transcription, signal transduction, and RNA processing. Overexpression of PRMT1 is related to cardiovascular diseases, kidney diseases, and cancers; therefore, selective PRMT1 inhibitors serve as chemical probes to investigate the biological function of PRMT1 and drug candidates for disease treatment. Our previous work found trimethine cyanine compounds that effectively inhibit PRMT1 activity. In our present study, we systematically investigated the structure–activity relationship of cyanine structures. A pentamethine compound, E-84 (compound 50), showed inhibition on PRMT1 at the micromolar level and 6- to 25-fold selectivity over CARM1, PRMT5, and PRMT8. The cellular activity suggests that compound 50 permeated the cellular membrane, inhibited cellular PRMT1 activity, and blocked leukemia cell proliferation. Additionally, our molecular docking study suggested compound 50 might act by occupying the cofactor binding site, which provided a roadmap to guide further optimization of this lead compound. PMID:25559100

  13. Synthesis, Structures and Properties of Cobalt Thiocyanate Coordination Compounds with 4-(hydroxymethylpyridine as Co-ligand

    Directory of Open Access Journals (Sweden)

    Stefan Suckert

    2016-04-01

    Full Text Available Reaction of Co(NCS2 with 4-(hydroxymethylpyridine (hmpy leads to the formation of six new coordination compounds with the composition [Co(NCS2(hmpy4] (1, [Co(NCS2(hmpy4] × H2O (1-H2O, [Co(NCS2(hmpy2(EtOH2] (2, [Co(NCS2(hmpy2(H2O2] (3, [Co(NCS2(hmpy2]n∙4 H2O (4 and [Co(NCS2(hmpy2]n (5. They were characterized by single crystal and powder X-ray diffraction experiments, thermal and elemental analysis, IR and magnetic measurements. Compound 1 and 1-H2O form discrete complexes, in which the Co(II cations are octahedrally coordinated by two terminal thiocyanato anions and four 4-(hydroxymethylpyridine ligands. Discrete complexes were also observed for compounds 2 and 3 where two of the hmpy ligands were substituted by solvent, either water (3 or ethanol (2. In contrast, in compounds 4 and 5, the Co(II cations are linked into chains by bridging 4-(hydroxymethylpyridine ligands. The phase purity was checked with X-ray powder diffraction. Thermogravimetric measurements showed that compound 3 transforms into 5 upon heating, whereas the back transformation occurs upon resolvation. Magnetic measurements did not show any magnetic exchange via the hmpy ligand for compound 5.

  14. Design, Synthesis, and Biological Activities of Novel Pyrazole Oxime Compounds Containing a Substituted Pyridyl Moiety

    Directory of Open Access Journals (Sweden)

    Cuili Chen

    2017-05-01

    Full Text Available In this paper, in order to find novel biologically active pyrazole oximes, a series of pyrazole oxime compounds bearing a substituted pyridyl unit were prepared. Bioassays showed that some target compounds were found to have good acaricidal activity against Tetranychus cinnabarinus at a concentration of 500 μg/mL, compound 9q especially displayed potent acaricidal activity against T. cinnabarinus when the concentration was reduced to 100 μg/mL. Interestingly, most target compounds possessed excellent insecticidal activities against Oriental armyworm at 500 μg/mL. Moreover, some compounds were active against Aphis medicaginis and Nilaparvata lugens at 500 μg/mL. Additionally, compounds 9b, 9g, 9l, 9p, 9q, 9r, 9s, 9t, 9u, and 9v displayed significant antiproliferative activities against HepG2 cells with IC50 values of 1.53–17.27 μM, better than that of the control 5-fluorouracil (IC50 = 35.67 μM.

  15. Three new bismuth(III) pyridine-2,6-dicarboxylate compounds: Synthesis, characterization and crystal structures

    Science.gov (United States)

    Hakimi, Mohammad; Motieiyan, Elham; Bertolotti, Federica; Marabello, Domenica; Nunes Rodrigues, Vitor Hugo

    2015-11-01

    Three new metal-organic compounds containing bismuth and pyridine-2,6-dicarboxylate (pydc) formulated as (2-apyH)2[Bi(pydc)2(pydcH)]·2H2O, 1, (4-apyH)[Bi(pydc) (pydcH)2].4H2O, 2 and (pipzeaH)[Bi2(pydc)3(pydcH) (H2O)2]·5H2O, 3, (2-apy = 2-aminopyridine, 4-apy = 4-aminopyridine, pipzea = 2-piperazin-1-ylethanamine), have been synthesized in deionized water and characterized by elemental analysis (C, H and N), spectral (UV-Vis, IR), 1H NMR spectroscopy, TGA and single crystal X-ray diffraction. These compounds were obtained via proton transfer methodology. Compounds 1 and 2 have similar monomeric bismuth coordination units, whereas compound 3 has a dimeric bismuth coordination unit. The compounds are anionic in 1 and 2 and they are connected non-covalently to 2-apyH and 4-apyH, respectively. In 3, two molecules are present, one neutral and one anionic, and both are connected non-covalently to pipzeaH cations. Five different coordination modes of Bi-pydc exist in 1, 2 and 3. These compounds are stabilized in the solid state by a complex network of hydrogen bonds between crystallization water molecules, anionic, cationic and neutral fragments, forming 3D-supramolecular arrays.

  16. Differential methods of inoculation of plant growth-promoting rhizobacteria induce synthesis of phenylalanine ammonia-lyase and phenolic compounds differentially in chickpea.

    Science.gov (United States)

    Basha, S A; Sarma, B K; Singh, D P; Annapurna, K; Singh, U P

    2006-01-01

    Foliar spray and micro-injection of plant growth-promoting rhizobacterial species, viz. Pseudomonas fluorescens and P. aeruginosa on chickpea induced synthesis of phenylalanine ammonia-lyase (PAL) when tested against Sclerotinia sclerotiorum. Induction of PAL was also associated with increased synthesis of phenolic compounds such as tannic, gallic, caffeic, chlorogenic and cinnamic acids. Treatment with P. fluorescens was found to be more effective in inducing phenolic compounds as compared to P. aeruginosa. However, persistence of PAL activity was observed more with P. aeruginosa. Although both the inoculation methods were effective, foliar application was found to be superior to micro-injection in terms of rapid PAL activity leading to the synthesis of phenolic compounds.

  17. Synthesis of new 4-methyl-2-(4-pyridyl)-1,2,3,4-tetrahydroquinolines as potent antifungal compounds

    Energy Technology Data Exchange (ETDEWEB)

    Mendez, Leonor Y. Vargas [Universidad Santo Tomas, Bucaramanga (Colombia). Grupo de Investigaciones Ambientales; Zacchino, Susana A. [Universidad Nacional del Rosario, (Argentina). Lab. de Farmacognosia; Kouznetsov, Vladimir V. [Universidad Industrial de Santander, Bucaramanga (Colombia). Lab. de Quimica Organica y Biomolecular

    2010-07-01

    Synthesis, spectral characterization and biological results of new series of 2-(4-pyridyl)- 1,2,3,4-tetrahydroquinolines and their closer precursors, -N-aryl-N-[1-(4-pyridyl)but-3-enyl] amines are reported. It was found that both g-pyridyl substituted precursors and final products, tetrahydroquinolines, showed very good antifungal activities against Aspergillus fumigatus, Aspergillus flavus, Aspergillus niger, Microsporum gypseun, Trichophyton rubrum and Trichophyton mentagrophytes. (author)

  18. Reduction of nitrogen compounds in oceanic basement and its implications for HCN formation and abiotic organic synthesis

    Directory of Open Access Journals (Sweden)

    Neubeck Anna

    2009-10-01

    Full Text Available Abstract Hydrogen cyanide is an excellent organic reagent and is central to most of the reaction pathways leading to abiotic formation of simple organic compounds containing nitrogen, such as amino acids, purines and pyrimidines. Reduced carbon and nitrogen precursor compounds for the synthesis of HCN may be formed under off-axis hydrothermal conditions in oceanic lithosphere in the presence of native Fe and Ni and are adsorbed on authigenic layer silicates and zeolites. The native metals as well as the molecular hydrogen reducing CO2 to CO/CH4 and NO3-/NO2- to NH3/NH4+ are a result of serpentinization of mafic rocks. Oceanic plates are conveyor belts of reduced carbon and nitrogen compounds from the off-axis hydrothermal environments to the subduction zones, where compaction, dehydration, desiccation and diagenetic reactions affect the organic precursors. CO/CH4 and NH3/NH4+ in fluids distilled out of layer silicates and zeolites in the subducting plate at an early stage of subduction will react upon heating and form HCN, which is then available for further organic reactions to, for instance, carbohydrates, nucleosides or even nucleotides, under alkaline conditions in hydrated mantle rocks of the overriding plate. Convergent margins in the initial phase of subduction must, therefore, be considered the most potent sites for prebiotic reactions on Earth. This means that origin of life processes are, perhaps, only possible on planets where some kind of plate tectonics occur.

  19. A Terpene Synthase Is Involved in the Synthesis of the Volatile Organic Compound Sodorifen of Serratia plymuthica 4Rx13.

    Science.gov (United States)

    Domik, Dajana; Thürmer, Andrea; Weise, Teresa; Brandt, Wolfgang; Daniel, Rolf; Piechulla, Birgit

    2016-01-01

    Bacteria release a plethora of volatile organic compounds, including compounds with extraordinary structures. Sodorifen (IUPAC name: 1,2,4,5,6,7,8-heptamethyl-3-methylenebicyclo[3.2.1]oct-6-ene) is a recently identified and unusual volatile hydrocarbon that is emitted by the rhizobacterium Serratia plymuthica 4R×13. Sodorifen comprises a bicyclic ring structure solely consisting of carbon and hydrogen atoms, where every carbon atom of the skeleton is substituted with either a methyl or a methylene group. This unusual feature of sodorifen made a prediction of its biosynthetic origin very difficult and so far its biosynthesis is unknown. To unravel the biosynthetic pathway we performed genome and transcriptome analyses to identify candidate genes. One knockout mutant (SOD_c20750) showed the desired negative sodorifen phenotype. Here it was shown for the first time that this gene is indispensable for the synthesis of sodorifen and strongly supports the hypothesis that sodorifen descends from the terpene metabolism. SOD_c20750 is the first bacterial terpene cyclase isolated from Serratia spp. and Enterobacteriales. Homology modeling revealed a 3D structure, which exhibits a functional role of amino acids for intermediate cation stabilization (W325) and putative proton acception (Y332). Moreover, the size and hydrophobicity of the active site strongly indicates that indeed the enzyme may catalyze the unusual compound sodorifen.

  20. A terpene synthase is involved in the synthesis of the volatile organic compound sodorifen of Serratia plymuthica 4Rx13

    Directory of Open Access Journals (Sweden)

    Dajana eDomik

    2016-05-01

    Full Text Available Bacteria release a plethora of volatile organic compounds (VOCs, including compounds with extraordinary structures. Sodorifen (IUPAC name: 1,2,4,5,6,7,8-heptamethyl-3-methylenebicyclo[3.2.1]oct-6-ene is a recently identified and unusual volatile hydrocarbon that is emitted by the rhizobacterium Serratia plymuthica 4Rx13. Sodorifen comprises a bicyclic ring structure solely consisting of carbon and hydrogen atoms, where every carbon atom of the skeleton is substituted with either a methyl or a methylene group. This unusual feature of sodorifen made a prediction of its biosynthetic origin very difficult and so far its biosynthesis was unknown. To unravel the biosynthetic pathway we performed genome and transcriptome analyses to identify candidate genes. One knockout mutant (SOD_c20750 showed the desired negative sodorifen phenotype. Here it was shown for the first time that this gene is indispensable for the synthesis of sodorifen and strongly supports the hypothesis that sodorifen descends from the terpene metabolism. SOD_c20750 is the first bacterial terpene cyclase isolated from Serratia spp. and Enterobacteriales. Homology modeling revealed a 3D structure, which indicated a functional role of amino acids for intermediate cation stabilization (W325 and putative proton acceptance (Y331. Moreover, the size and hydrophobicity of the active site strongly indicated that indeed the enzyme may catalyze the unusual compound sodorifen.

  1. In Situ Synthesis of Titanium Nickel Intermetallic Compounds Layer and TiN Coating By Laser Cladding

    Institute of Scientific and Technical Information of China (English)

    ZHANG Cui-hong; YANG Yong-qiang; XU Wei-hong

    2006-01-01

    Laser cladding,together with laser nitriding was used to synthesize a titanium nickel intermetallic compound layer on the nickel substrate and a TiN coating on the cladding layer. During the laser cladding, Ti and Ni powders were blown into the melting pool by a six-hole coaxial nozzle powder injection system. Exothermic reactions between Ti and Ni took place in the melting pool, and a cladding layer of titanium nickel intermetallic compounds was produced. Laser nitriding in a nitrogen-rich atmosphere followed the production of the cladding layer, and formed a golden yellow TiN layer over it. An optical and a scanning electron microscope were used to investigate the microstructures and measure the thicknesses of the cladding layer and the TiN layer. Phase identification was carried out by XRD. For the nitriding sample, the microhardness profile of the clad layer was tested. The optimal process parameters of the in situ synthesis of titanium nickel intermetallic compounds were obtained.

  2. CASE REPORT OF COMPOUND COMMINUTED FRACTURE CLAVICLE WITH VEIN AND PLEURAL INJURY

    Directory of Open Access Journals (Sweden)

    Vinayak Nerlikar

    2015-01-01

    Full Text Available We report a case of compound segmental comminuted fracture of the Left clavicle , fracture of second rib , comminuted fracture of scapula with subclavian vein laceration and perforation of the parietal pleura and lung contusion that caused massive haemo - pneumothorax. Emergency exploration followed by repair of subclavian vein , pleura and fixation of clavicle were able to salvage the patient.

  3. Detection of estrogenic activity in sediment-associated compounds using in vitro reporter gene assays

    NARCIS (Netherlands)

    Legler, J.; Dennekamp, M.; Vethaak, A.D.; Brouwer, A.; Koeman, J.H.; Burg, van der B.; Murk, A.J.

    2002-01-01

    Sediments may be the ultimate sink for persistent (xeno-) estrogenic compounds released into the aquatic environment. Sediment-associated estrogenic potency was measured with an estrogen receptor-mediated luciferase reporter gene (ER-CALUX) assay and compared with a recombinant yeast screen. The ER-

  4. FINAL REPORT: MEMBRANE-MEDIATED EXTRACTION AND BIODEGRADATION OF VOLATILE ORGANIC COMPOUNDS FROM AIR

    Science.gov (United States)

    The report describes feasibility tests of a two-step strategy for air pollution control applicable to exhaust air contaminated with volatile organic compounds (VOCs) from painting aircraft. In the first step, the VOC-contaminated air passes over coated, polypropylene, hollow-fibe...

  5. Detection of estrogenic activity in sediment-associated compounds using in vitro reporter gene assays

    NARCIS (Netherlands)

    Legler, J.; Dennekamp, M.; Vethaak, A.D.; Brouwer, A.; Koeman, J.H.; Burg, van der B.; Murk, A.J.

    2002-01-01

    Sediments may be the ultimate sink for persistent (xeno-) estrogenic compounds released into the aquatic environment. Sediment-associated estrogenic potency was measured with an estrogen receptor-mediated luciferase reporter gene (ER-CALUX) assay and compared with a recombinant yeast screen. The ER-

  6. [Synthesis and antitumor activity of 5-substituted-2-(pyridyl)benzothiazole compounds].

    Science.gov (United States)

    Liu, Wen-Hu; Chang, Jin-Xia; Liu, Yi

    2013-01-01

    Fifteen novel 5-substituted-2-(pyridyl)benzothiazole compounds were designed and synthesized by simple hydrolization and condensation reaction of the 2-amino-5-substituent benzothiazole. Activities of these synthesized compounds were evaluated on Bcap-37, HCT-15 and HepG2 tumor cells in vitro by standard MTT assay. 5-Fluorouracil (5-FU) was used as the positive control. The results revealed that most of the new compounds had potent effects on Bcap-37, HCT-15 and HepG2 tumor cells, and had no or less effect on 293T and L02 normal cells. Particularly, compounds 1c and 2e exhibited better activities on HCT-15 and HepG2 cells with IC50 values of 41.59 and 38.65 micromol x L(-1), and 1i showed excellent activities on Bcap-37 and HepG2 cells with IC50 values of 46.63 and 23.51 micromol x L(-1), respectively. The structure-activity relationship of 5-substituted-2-(pyridyl)benzothiazole compounds were also discussed preliminarily.

  7. Synthesis of 1S-ethyl-4-substituted quinolizidines and other potentially bioactive compounds

    OpenAIRE

    2012-01-01

    [eng] A dissertation submitted by Vladislav SEMAK to obtain a doctoral degree from University of Barcelona. This thesis was developed under the supervision of Dr. Carmen Escolano Mirón from Faculty of Pharmacy, University of Barcelona. This doctoral thesis is presented as a compendium of publications. The thesis is divided in four chapters: CHAPTER 1 – PART A: Enantioselective, Protecting Group-Free Synthesis of 1S-Ethyl-4-Substituted Quinolizidines (Amat, M.; Semak, V.; Escolano, C....

  8. Enzymatic synthesis of bioactive compounds by Rhus laccase from Chinese Rhus vernicifera

    Institute of Scientific and Technical Information of China (English)

    WAN YunYang; LU Rong; AKIYAMA Kazuhiro; MIYAKOSHI Tetsuo; DU YuMin

    2007-01-01

    A simple one step synthesis of pinoresinol and its derivatives-active components of Du-Zhong (Eucommia ulmoides)-from coniferyl alcohol and p-courmaryl alcohol with higher yields was achieved by Rhus laccases (RL) catalysis in water miscible organic solvents. Biomacromolecules dehydrogenative polymers (DHP) were only synthesized by fungal laccases, not by RL. The structures and the reaction mechanism were discussed to promote the understanding of the function of laccases in the process of lignin biosynthesis.

  9. THE EFFECT OF A NEW SALICYLIC ACID SYNTHESIS COMPOUNDS ADMINISTRATION ON SERUM TRANSAMINASIS

    OpenAIRE

    LETIŢIA STANA

    2013-01-01

    The chemical synthesis product is the amide of chlorine salicylic acid andsulphanilamide (5ClSA-SA). This research had as objective the effect of this productfrom salicylic acid class as a potential medicine on the serum transaminasis activity.5ClSA-SA has been administrated intraperitoneal to Wistar rats for 7 daysconsecutively determining ALT and AST transaminasis activities after 5 and 7 days.Serum transaminases had high values compared to the control sample (220% ASTand 237% ALT).This syn...

  10. An expedient synthesis of functionalized 1,4-diketone-derived compounds via silyloxyallyl cation intermediates.

    Science.gov (United States)

    Stepherson, Jacob R; Fronczek, Frank R; Kartika, Rendy

    2016-02-07

    Herein we describe a new method, enabling the synthesis of highly functionalized 1,4-diketones that are readily differentiated as monosilylenol ethers under Brønsted acid catalysis. This synthetically useful chemistry exploited an intermediacy of unsymmetrical silyloxyallyl cations, which were directly captured by silyl enolates to create the targeted α,α carbon-carbon linkages in a regioselective manner. Our reaction conditions proved to be mild, rendering the silylenol ether functionalities intact.

  11. Synthesis, Characterization, and Antimicrobial Activities of Coordination Compounds of Aspartic Acid

    Directory of Open Access Journals (Sweden)

    T. O. Aiyelabola

    2016-01-01

    Full Text Available Coordination compounds of aspartic acid were synthesized in basic and acidic media, with metal ligand M : L stoichiometric ratio 1 : 2. The complexes were characterized using infrared, electronic and magnetic susceptibility measurements, and mass spectrometry. Antimicrobial activity of the compounds was determined against three Gram-positive and three Gram-negative bacteria and one fungus. The results obtained indicated that the availability of donor atoms used for coordination was a function of the pH of the solution in which the reaction was carried out. This resulted in varying geometrical structures for the complexes. The compounds exhibited a broad spectrum of activity and in some cases better activity than the standard.

  12. Synthesis, Structure and Properties of Two Photochromic Compounds Containing A Pyrazolone-ring

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Two photochromic compounds with the pyrazolone-ring as the photochromic functional structure, 2-(1'-phenyl-3'-methyl-4'-benzoformyl-pyrazolone-5')-thiosemicarbazone(PMBP-TSC) and 2-(1'-phenyl-3'-methyl-4'-benzoformyl-pyrazolone-5')-S-methylthiosemicarbazone(PMBP-MTSC), were synthesized and characterized by elemental analysis, MS, IR spectra, NMR spectra. The crystal structure of the photocolored product of PMBP-TSC was determined by single crystal XRD analysis. The results show that the photochromic phenomenon is due to the photoisomerization from enol form to keto form. Their photochromic properties were studied by powder-UV reflectance spectra under the irradiation of 200-380 nm light. The first-order rate constants of the photocoloring reaction were found to be 7.80×10-3 s-1 for compound 1A and 1.03×10-3 s-1 for compound 2A.

  13. Synthesis and crystal structures of coordination compounds of pyridoxine with zinc and cadmium sulfates

    Science.gov (United States)

    Furmanova, N. G.; Berdalieva, Zh. I.; Chernaya, T. S.; Resnyanskiĭ, V. F.; Shiitieva, N. K.; Sulaĭmankulov, K. S.

    2009-03-01

    The pyridoxine complexes with zinc and cadmium sulfates are synthesized. The IR absorption spectra and thermal behavior of the synthesized compounds are described. Crystals of the [ M(C8H11O3N)2(H2O)2]SO4 · 3H2O ( M = Zn, Cd) compounds are investigated using X-ray diffraction. In the structures of both compounds, the M atoms are coordinated by the oxygen atoms of the deprotonated OH group and the CH2OH group retaining its own hydrogen atom, as well as by two H2O molecules, and have an octahedral coordination. The nitrogen atom of the heterocycle is protonated, so that the heterocycle acquires a pyridinium character. The cationic complexes form layers separated by the anions and crystallization water molecules located in between. The structural units of the crystals are joined together by a complex system of hydrogen bonds.

  14. Synthesis and TFT Properties of Fluorenyl Cored Conjugated Compound for Organic Thin Film Transistors.

    Science.gov (United States)

    Kim, You Geun; Shaik, Baji; Jang, Yong Ju; Park, Song Yi; Kim, Jin Young; Lee, Sang-Gyeong

    2016-03-01

    The 5,5'-(4,4'-(9,9-dioctyl-9H-fluorene-2,7-diyl)bis(4,1-phenylene))bis(2-hexylthieno[3,2-b]thiophene) FCBT (6) was synthesized by connecting the fluorenyl, thienothiophenyl and phenyl units. The compound was characterized by FT-IR, H1NMR, C13NMR and mass spectroscopy. The compound has shown good solubility and thermal stability over 417 degrees C. The compound has shown hole mobility of 4.76 x 10(-6) cm2Ns. The on-off ratio and threshold voltage were 7.5 x 10(2) and -8.26 V respectively.

  15. Synthesis and evaluation of some bioactive compounds having oxygen and nitrogen heteroatom

    Indian Academy of Sciences (India)

    Poonam Yadav; Nalini V Purohit

    2013-01-01

    Some new 3,4-disubstituted isocoumarins were synthesized having bioactive pyrazole molecule at 3rd position of isocoumarin moiety (5a,b), from isocoumarin -3- carboxylic acid hydrazide (4a,b) followed by cyclization with acetyl acetone. A series of isocoumarin derivative having Schiff base as lateral side chain at 3rd position of isocoumarin moiety were also synthesized (7a,b), by condensing isocoumarin acid hydrazide and benzaldehyde derivative followed by dehydration. The chemical structures of all the compounds were determined by analytical and spectral method. The lead compounds were screened for antimicrobial and analgesic activities.

  16. New macrocyclic compounds using organotin complexes as intermediates: synthesis and characterization

    Directory of Open Access Journals (Sweden)

    Harminder Kaur

    2012-06-01

    Full Text Available Background & Aim:A new series of macrocyclic compounds 1-4 have been synthesized using tin as templates.Method:Tin templates are formed by refluxing the solution of dibutyltin (IV oxide with orthophenylenediamine (L1H,4-chlorocatechol (L2H, butane dithiol (L3H and 3-carboxypropyldisulphide (L4H. Results:The reaction is visualizedby cleavage X-Sn-X (X= oxygen/ nitrogen/ sulphur atom bond of tin template when treated withadipoyldichloride. Conclusion:The compounds 1-4 are characterized with the aid of elemental analyses, IR and NMR(1H, 13C studies which confirmed their proposed framework.

  17. [Development of novel methods for synthesis of heterocyclic compounds catalyzed by transition metals in fluorinated alcohols].

    Science.gov (United States)

    Saito, Akio

    2008-08-01

    New possibilities for catalytic syntheses of lactone derivatives and nitrogen-containing heterocyclic compounds in fluorinated alcohols are described. The cationic Rh(I) catalyst in fluorinated alcohol solvents (hexafluoroisopropanol: HFIP, trifluoroethanol: TFE) brought about not only mild cycloaddition reactions of ester-tethered compounds but also a facile formation of indole derivatives by the aromatic amino-Claisen rearrangement of N-propargyl aniline derivatives. The use of HFIP as an additive exerted a remarkable effect on the Pictet-Spengler reaction catalyzed by the fluorinated surfactant-combined Brønsted acid catalyst in water.

  18. Design, synthesis and cytotoxic activity of some novel compounds containing pyrazolo[3,4-]pyrimidines nucleus

    Indian Academy of Sciences (India)

    Manal M Kandeel; Sameha M Roshdy; Eman K A Abdelall; Mohamed A Abdelgawad; Phoebe F Lamie

    2013-09-01

    Novel pyrazolo[3,4-]pyrimidines were designed and synthesized as antitumour agents against human breast cancer adenoma (MCF-7). Molecular modelling and pharmacological screening were performed against breast cancer cell line and also certain synthetic pathways were developed in order to introduce functionality onto C6 and N5 positions of pyrimidine moiety. Surprisingly, all the test compounds showed IC50 lower than that of the standard olomoucine I, especially compounds 4b, 8a, 10b, 11a and b, which showed IC50 between 0.009 and 0.004 M.

  19. An Efficient One-pot Synthesis of β-Amino/β-Acetamido Car-bonyl Compounds via ZrCl4-catalyzed Mannich-type Reaction

    Institute of Scientific and Technical Information of China (English)

    SANJEEVA REDDY,Cherkupally; PURNACHANDRA REDDY,Gurrala

    2008-01-01

    Zirconium(IV) chloride catalyzed efficient one-pot synthesis of β-amino/β-acetamido carbonyl compounds at room temperature is described. In the presence of ZrCl4, the three-component Mannich-type reaction via a variety of in situ generated aldimines, with various ketones, aromatic aldehydes and aromatic amines in ethanol, led to the formation of β-amino carbonyl compounds and the four-component Mannich-type reaction of aromatic aldehydes with various ketones, acetonitrile and acetyl chloride resulted in the corresponding β-acetamido carbonyl com-pounds in high to excellent yields. This methodology has also been applied towards the synthesis of dimeric β-amino/β-acetamido carbonyl compounds.

  20. Redirecting photosynthetic electron flow into light-driven synthesis of alternative products including high-value bioactive natural compounds.

    Science.gov (United States)

    Lassen, Lærke Münter; Nielsen, Agnieszka Zygadlo; Ziersen, Bibi; Gnanasekaran, Thiyagarajan; Møller, Birger Lindberg; Jensen, Poul Erik

    2014-01-17

    Photosynthesis in plants, green algae, and cyanobacteria converts solar energy into chemical energy in the form of ATP and NADPH, both of which are used in primary metabolism. However, often more reducing power is generated by the photosystems than what is needed for primary metabolism. In this review, we discuss the development in the research field, focusing on how the photosystems can be used as synthetic biology building blocks to channel excess reducing power into light-driven production of alternative products. Plants synthesize a large number of high-value bioactive natural compounds. Some of the key enzymes catalyzing their biosynthesis are the cytochrome P450s situated in the endoplasmic reticulum. However, bioactive compounds are often synthesized in low quantities in the plants and are difficult to produce by chemical synthesis due to their often complex structures. Through a synthetic biology approach, enzymes with a requirement for reducing equivalents as cofactors, such as the cytochrome P450s, can be coupled directly to the photosynthetic energy output to obtain environmentally friendly production of complex chemical compounds. By relocating cytochrome P450s to the chloroplasts, reducing power can be diverted toward the reactions catalyzed by the cytochrome P450s. This provides a sustainable production method for high-value compounds that potentially can solve the problem of NADPH regeneration, which currently limits the biotechnological uses of cytochrome P450s. We describe the approaches that have been taken to couple enzymes to photosynthesis in vivo and to photosystem I in vitro and the challenges associated with this approach to develop new green production platforms.

  1. Microwave-assisted synthesis of antimicrobial dihydropyridines and tetrahydropyrimidin-2-ones: novel compounds against aspergillosis.

    Science.gov (United States)

    Chhillar, Anil K; Arya, Pragya; Mukherjee, Chandrani; Kumar, Pankaj; Yadav, Yogesh; Sharma, Ajendra K; Yadav, Vibha; Gupta, Jyotsana; Dabur, Rajesh; Jha, Hirday N; Watterson, Arthur C; Parmar, Virinder S; Prasad, Ashok K; Sharma, Gainda L

    2006-02-15

    Ten 4-aryl-1,4-dihydropyridine and three 4-aryl-1,2,3,4-tetrahydropyrimidin-2-one derivatives have been synthesized and examined for their activity against pathogenic strains of Aspergillus fumigatus and Candida albicans. Although none of the three compounds belonging to pyrimidin-2-one series showed any activity against two pathogens, two of the compounds of the dihydropyridine series, that is, diethyl 4-(4-methoxyphenyl)-2,6-dimethyl-1,4-dihydropyridin-3,5-dicarboxylate and dimethyl 4-(4-methoxyphenyl)-2,6-dimethyl-1,4-dihydropyridin-3,5-dicarboxylate, exhibited significant activity against A. fumigatus in disc diffusion, microbroth dilution and percent spore germination inhibition assays. The most active diethyl dihydropyridine derivative exhibited a MIC value of 2.92 microg/disc in disc diffusion and 15.62 microg/ml in microbroth dilution assays. The MIC(90) value of the most active compound by percent germination inhibition assay was found to be 15.62 microg/ml. The diethyl dicarboxylate derivative of dihydropyridine also exhibited appreciable activity against C. albicans. The in vitro toxicity of the most active diethyl dihydropyridine derivative was evaluated using haemolytic assay, in which the compound was found to be non-toxic to human erythrocytes even at a concentration of 625 microg/ml. The standard drug amphotericin B exhibited 100% lysis of erythrocytes at a concentration almost 16 times less than the safer concentration of the most active dihydropyridine derivative.

  2. Synthesis and structural characterization of new inorganic–organic hybrid: arsenomolybdate compound with cytosinium cations

    Indian Academy of Sciences (India)

    Meriem Ayed; Brahim Ayed; Amor Haddad

    2015-02-01

    New organic–inorganic hybrid compound, with formula (C4H6N3O)6 [(HAsO4)2Mo6O19].7H2O, was prepared and characterized by IR and UV–visible spectroscopies and X-ray diffraction techniques. Thermal analysis was performed to study their thermal stability. The crystal structure of the title compound (triclinic, space group $P − 1$, = 2) was determined by X-ray diffraction. The compound contains the polyanion [(HAsO4)2Mo6O19]6−, which consists of the six molybdenum octahedral grouped into two parts consisting of four edge-sharing octahedral and two face-sharing octahedral, respectively, these two parts are connected by two corner-sharing O atoms to form a bent Mo6 ring. The polyanion framework derives from the Strandberg type and it is a new isomer. The cytosinium cations (Cyt+) are embedded in the channels and interact with the inorganic framework by way of N-H $\\cdots$ O and O-H $\\cdots$ O hydrogen bonds. Furthermore, the electrochemical property of this compound has been studied.

  3. Thorium Compounds with Bonds to Sulfur or Selenium: Synthesis, Structure, and Thermolysis.

    Science.gov (United States)

    Rehe, David; Kornienko, Anna Y; Emge, Thomas J; Brennan, John G

    2016-07-18

    Thorium chalcogenolates Th(ER)4 (E = S, Se; R = Ph, C6F5) form pyridine complexes with a variety of coordination numbers. Four compounds, (py)4Th(SPh)4, (py)3Th(SePh)4, (py)3Th(SC6F5)4, and (py)4Th(SeC6F5)4, have been isolated and characterized by spectroscopic methods and low-temperature single crystal X-ray diffraction. Two of the products, (py)4Th(SPh)4 and (py)4Th(SeC6F5)4, have classic eight coordinate A4B4 square-antiprism geometries. The SePh compound is the only seven coordinate (4Se, 3N) product, and the fluorinated thiolate is distinctive in that the structure contains two dative interactions between Th and fluoride, to give a nine coordinate (3N, 4S, 2F) structure. The EPh compounds decompose thermally to give ThE2 and EPh2, while the fluorinated compounds give primarily ThF4, E2(C6F5)2, and E(C6F5)2.

  4. Synthesis of Novel Fluorescence reagents and Their Application in Determination of Thiol Compounds

    Institute of Scientific and Technical Information of China (English)

    LIANG Shu-Cai; WANG Hong; ZHANG Hua-Shan; HU Xian-Ming

    2003-01-01

    @@ The identification and determination of thiol compounds is essential both for the clinical diagnosis and the con trol of diseases because alteration of their concentrations in biological systems are somehow responsive for some diseases such as myocardial infarction, diabetes, peripheral vascular and so on. [1

  5. Synthesis, Structure and Properties of Melamine-Based pTHF-Urethane Supramolecular Compounds

    NARCIS (Netherlands)

    Öjelund, Karin; Loontjens, Ton; Steeman, Paul; Palmans, Anja; Maurer, Frans

    2003-01-01

    The properties of melamine based supramolecular compounds have been studied with rheological, thermal, mechanical, dielectric and scattering techniques and compared with similar covalently bonded materials. The complexes are based on a linear pTHF-diol (M¯n=1 000) connected via a diisocyanate with m

  6. Dicarboxylic esters: Useful tools for the biocatalyzed synthesis of hybrid compounds and polymers

    Science.gov (United States)

    Bassanini, Ivan; Hult, Karl

    2015-01-01

    Summary Dicarboxylic acids and their derivatives (esters and anhydrides) have been used as acylating agents in lipase-catalyzed reactions in organic solvents. The synthetic outcomes have been dimeric or hybrid derivatives of bioactive natural compounds as well as functionalized polyesters. PMID:26664578

  7. Synthesis, structural characterization, and anticancer activity of a monobenzyltin compound against MCF-7 breast cancer cells

    Directory of Open Access Journals (Sweden)

    Fani S

    2015-11-01

    Full Text Available Somayeh Fani,1 Behnam Kamalidehghan,1 Kong Mun Lo,2 Najihah Mohd Hashim,1 Kit May Chow,2 Fatemeh Ahmadipour1 1Department of Pharmacy, Faculty of Medicine, 2Department of Chemistry, Faculty of Science, University of Malaya, Kuala Lumpur, Malaysia Abstract: A new monoorganotin Schiff base compound, [N-(3,5-dichloro-2-oxidobenzylidene-4-chlorobenzyhydrazidato](o-methylbenzylaquatin(IV chloride, (compound C1, was synthesized, and its structural features were investigated by spectroscopic techniques and single-crystal X-ray diffractometry. Compound C1 was exposed to several human cancer cell lines, including breast adenocarcinoma cell lines MCF-7 and MDA-MB-231, ovarian adenocarcinoma cell lines Skov3 and Caov3, and prostate cancer cell line PC3, in order to examine its cytotoxic effect for different forms of cancer. Human hepatic cell line WRL-68 was used as a normal cell line. We concentrated on the MCF-7 cell line to detect possible underlying mechanism involvement of compound C1. 3-(4,5-dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide (MTT assay revealed the strongest cytotoxicity of compound C1 against MCF-7 cells, with a half maximal inhibitory concentration (IC50 value of 2.5±0.50 µg/mL after 48 hours treatment. The IC50 value was >30 µg/mL in WRL-68 cells. Induced antiproliferative activity of compound C1 for MCF-7 cells was further confirmed by lactate dehydrogenase, reactive oxygen species, acridine orange/propidium iodide staining, and DNA fragmentation assays. A significant increase of lactate dehydrogenase release in treated cells was observed via fluorescence analysis. Luminescent analysis showed significant growth in intracellular reactive oxygen species production after treatment. Morphological changes of necrosis and early and late apoptosis stages were observed in treated cells after staining with acridine orange/propidium iodide. DNA fragmentation was observed as a characteristic of apoptosis in treated cells. Results of the

  8. Synthesis and antioxidant activity of two novel tetraphenolic compounds derived from toluhydroquinone and tertiary butylhydroquinone

    Directory of Open Access Journals (Sweden)

    Jiang, Z. W.

    2014-06-01

    Full Text Available Two novel compounds bearing four hydroxyphenyl groups were synthesized by the acid-catalyzed condensation reaction of glyoxal with toluhydroquinone (THQ or tertiary butylhydroquinone (TBHQ, respectively. The antioxidant activity of the newly synthesized compounds was assessed by the Rancimat test, a 2,2-diphenyl 1-picrylhydrazyl (DPPH assay and reducing power assay. In the Rancimat antioxidant test using lard oil as substrate, the performance of two newly synthesized compounds was superior to TBHQ at 140 °C. It was suggested that two newly synthesized compounds can be used to improve the oxidative stability of lipid products during high temperature processing. With regard to the DPPH radical scavenging activity and reducing power, the performance of synthesized compounds was inferior to their mother compounds, respectively. The results show that the DPPH radical scavenging activity and reducing power of a compound did not correlate with its ability to retard lipid oxidation.Dos nuevos compuestos con cuatro grupos hidroxifenilo se sintetizaron mediante reacción de condensación catalizada por glioxal con toluhidroquinona (THQ o terbutilhidroquinona (TBHQ, respectivamente. La actividad antioxidante de los compuestos sintetizados se evaluó mediante Rancimat, método del 2,2-difenil-1-picrilhidrazil (DPPH y poder reductor. Para el ensayo de Rancimat se usó manteca de cerdo como sustrato, la efectividad de los dos compuestos recién sintetizados fue superior a la del TBHQ a 140 °C. Se sugiere que los compuestos sintetizados se pueden utilizar para mejorar la estabilidad oxidativa de productos lipídicos durante el procesamiento a alta temperatura. Con respecto a la actividad de eliminación de radicales DPPH y poder reductor, la efectividad de los compuestos sintetizados fue inferior a los compuestos matrices. Los resultados mostraron que la actividad de eliminación de radicales DPPH y poder reductor de un compuesto no se correlacionó con su

  9. Synthesis and light-emitting properties of organic electroluminescent compounds and their metal complexes

    Institute of Scientific and Technical Information of China (English)

    CUI Jianzhong; Kim Sung-Hoon

    2004-01-01

    Several organic electroluminescent (EL) compounds, 2,2′-(1,4-phenylenedivinylene)bis-3,3-dimethyl-in- dolenine (1), 2,2′-(1,4-phenylenedivinylene)bis-benzoxazole (2), 2,2′-(1,4-phenylenedivinylene)bis-benzothiazole (3), 4,4′- (1,4-phenylenedivinylene)bis-quinoline (4), 2,2′-(1,4-phenyle- nedivinylene)bis-quinoline (5), 2,2′-(1,4-phenylenedivinyle- ne)bis-1,3,3-trimethyl-indolenine dichlo ride (6), 2,2′-(1,4- phenylene-divinylene)bis-1-hydro-3,3-dimethyl-indolenine dichloride (7), 2,2′-(1,4-phenylenedivinylene)bis-8-acetoxy- quinoline (8), 2,2′-(1,4-phenylenedivinylene)bis-8-hydroxyq- uinoline (9) and metal complexes of 9, Al(PHQ) (10) and Zn(PHQ) (11), have been synthesized and characterized. The crystal structure of 6 was determined. Light emitting properties of the prepared compounds have been investigated. 1 produces an orange-yellow emission (λmax = 575 nm). The cation, 6, gives a red emission (λmax = 607 nm), which is shifted 32 nm to the red compared to 1. 8 produces a yellow emission (λmax = 567 nm). The metal complex 10 gives a red emission (λmax = 610 nm), which is a red shift of 43 nm compared to 8. The change in structure in the prepared compound caused a change in the electron distribution in the compounds, which induces a large wavelength shift of the emitted-light. Thermal analysis showed that the decomposition temperatures of the metal complexes (10, 11) were higher than those for the smaller organic molecular compounds (1-9). Therefore, metal complexes (10, 11) can be used as EL materials over a larger temperature range.

  10. Combination multinitrogen with good oxygen balance: molecule and synthesis design of polynitro-substituted tetrazolotriazine-based energetic compounds.

    Science.gov (United States)

    He, Piao; Zhang, Jian-Guo; Wang, Kun; Yin, Xin; Zhang, Tong-Lai

    2015-06-01

    We investigated 5,8-dinitro-5,6,7,8-tetrahydrotetrazolo[1,5-b][1,2,4]triazine (short for DNTzTr (1)) using various ab initio quantum chemistry methods. We proposed an additional three novel polynitro-substituted tetrazolotriazine-based compounds with exceptional performance, including 5,8-dinitro-5,6-dioxotetrazolo[1,5-b][1,2,4]triazine, DNOTzTr (2), 4,5,9,10-tetranitro[1,2,4,5]tetrazolo[3,4-b][1,2,4,5]tetrazolo[3',4':5,6]triazino[2,3-e]triazine, TNTzTr (3), and 4,5,6,10,11,12-hexanitro-bis[1,2,4,5]tetrazolo[3',4':5,6]triazino[2,3-b:2',3'-e]triazine, HNBTzTr (4). The optimized structure, electronic density, natural bond orbital (NBO) charges and HOMO-LUMO orbitals, electrostatic potential on surface of molecule, IR- and NMR-predicted spectra, as well as thermochemical parameters were calculated with the B3LYP/6-311+G(2d) level of theory. Critical parameters such as density, enthalpy of formation (EOF), and detonation performance have also been predicted. Characters with positive EOF (1386.00 and 1625.31 kJ/mol), high density (over 2.00 g/cm(3)), outstanding detonation properties (D = 9.82 km/s, P = 45.45 GPa; D = 9.94 km/s, P = 47.30 GPa), the perfect oxygen balance set to zero, and acceptable impact sensitivity led novel compounds 3 and 4 to be very promising energetic materials. This work provides the theoretical molecule design and a reasonable synthesis path for further experimental synthesis and testing.

  11. [Prevention of the eruption of an upper later incisor by a compound odontoma. Case report].

    Science.gov (United States)

    Vlcek, Daniel; Reichart, Peter A; Bosshardt, Dieter D; Sleiter, Roberto; Bornstein, Michael M

    2012-01-01

    Odontomas are the most common odontogenic tumours. They are considered as hamartomas - a local tissue malformation without autonomous growth potential - and are non-neoplastic. Clinically and histopathologically, compound and complex odontomas can be differentiated. Compound odontomas consist of a varying number of tooth-like structures and histology show dental tissues in an orderly pattern. Most often compound odontomas are diagnosed in young patients in the anterior maxilla. Patients are rarely complaining of symptoms and they are usually diagnosed during routine radiographic examinations or due to late eruption of permanent or persistence of deciduous teeth. The following case report presents a disturbed eruption of a lateral right incisor of the maxilla in a 8-year old female patient. Clinical, radiological and histopathological characteristics of this lesion will be discussed as well as therapy and follow-up.

  12. Polycyclic Aromatic Compounds as Anticancer Agents: Synthesis and Biological Evaluation of Methoxy Dibenzofluorene Derivatives

    Directory of Open Access Journals (Sweden)

    Bimal Krishna Banik

    2014-08-01

    Full Text Available Synthesis of a new methoxy dibenzofluorene through alkylation, cyclodehydration and aromatization in a one-pot operation is achieved for the first time. Using this hydrocarbon, a few derivatives are prepared through aromatic nitration, catalytic hydrogenation, coupling reaction with a side chain and reduction. The benzylic position of this hydrocarbon with the side chain is oxidized and reduced. Some of these derivatives have demonstrated excellent antitumor activities in vitro. This study confirms antitumor activity depends on the structures of the molecules.

  13. Enzymatic synthesis of bioactive compounds by Rhus laccase from Chinese Rhus vernicifera

    Institute of Scientific and Technical Information of China (English)

    AKIYAMA; Kazuhiro; MIYAKOSHI; Tetsuo

    2007-01-01

    A simple one step synthesis of pinoresinol and its derivatives-active components of Du-Zhong(Eu-commia ulmoides) -from coniferyl alcohol and p-courmaryl alcohol with higher yields was achieved by Rhus laccases(RL) catalysis in water miscible organic solvents. Biomacromolecules dehydro-genative polymers(DHP) were only synthesized by fungal laccases,not by RL. The structures and the reaction mechanism were discussed to promote the understanding of the function of laccases in the process of lignin biosynthesis.

  14. High-temperature electrochemical synthesis of carbon-containing inorganic compounds under excessive carbon dioxide pressure

    Directory of Open Access Journals (Sweden)

    Novoselova I.A.

    2003-01-01

    Full Text Available Features of the electroreduction of carbon dioxide dissolved in the equimolar melt of sodium and potassium chlorides under excessive pressure of up to 1.7 MPa have been studied by cyclic voltametry over a wide polarization rate range. It has been found that the electrode process occurs in two stages at sweep rates of ≤0.1 V s-1, and its mechanism has been suggested. The cathodic product is polycrystalline graphite. Systems and conditions for producing two- and three-component refractory metal carbides using CO2 as a synthesis component have been selected.

  15. Synthesis of acetylenic azomethines from imidoyl chlorides and copper(I) acetylides, catalyzed by palladium compounds

    Energy Technology Data Exchange (ETDEWEB)

    Ukhin, L.Yu.; Orlova, Zh.I.; Tokarskaya, O.A.

    1988-04-20

    The synthesis of acetylenic azomethines from N-phenylbenzimidoyl chloride and copper butylacetylide in the presence of lithium iodide, from imidoyl chlorides and copper and silver acetylides in boiling acetonitrile, and from imidoyl chloride and trimethylsilylacetylene with lead acetate and triphenylphosphine as catalyst (80/degree/C, 2 h) has been described. The authors have found that acetylenic azomethines are formed readily from imidoyl chlorides and copper acetylides at room temperature in the presence of the phosphine complexes of Pd(0), produced in situ.

  16. THE EFFECT OF A NEW SALICYLIC ACID SYNTHESIS COMPOUNDS ADMINISTRATION ON SERUM TRANSAMINASIS

    Directory of Open Access Journals (Sweden)

    LETIŢIA STANA

    2013-12-01

    Full Text Available sulphanilamide (5ClSA-SA. This research had as objective the effect of this productfrom salicylic acid class as a potential medicine on the serum transaminasis activity.5ClSA-SA has been administrated intraperitoneal to Wistar rats for 7 daysconsecutively determining ALT and AST transaminasis activities after 5 and 7 days. Serum transaminases had high values compared to the control sample (220% ASTand 237% ALT.This synthesis product can lead to stress that induces increasing of plasmaticenzymes activity, transaminasis being one of those.

  17. Climate and Land Use Change Effects on Ecological Resources in Three Watersheds: A Synthesis Report (Final Report)

    Science.gov (United States)

    EPA announced the availability of the final report, Climate and Land-Use Change Effects on Ecological Resources in Three Watersheds: A Synthesis Report. This report provides a summary of climate change impacts to selected watersheds and recommendations for how to improv...

  18. Equilibrium electrochemical synthesis diagrams of systems, forming homogeneous alloys and compounds

    Directory of Open Access Journals (Sweden)

    Kaptay G.

    2003-01-01

    Full Text Available In the present paper thermodynamic limitations will be derived and summarized in the form of Equilibrium Electrochemical Synthesis (EES diagrams, in order to predict the composition of the equilibrium phase, synthesized by galvanostatic co-deposition of components on inert electrodes. As a thermodynamic parameter, a difference of deposition potentials of pure components ( ∆E on inert cathodes is used (this parameter is a function of melt composition and temperature. Generally, the EES diagram predicts the equilibrium composition of the alloy as function temperature and ∆E. However, for systems with homogeneous alloy formation the composition- ∆E diagrams, drawn at a fixed temperature are more informative. As examples EES diagrams are constructed for the liquid Mg-Nd alloy, for some A(III-B(V (where A = Al, Ga, In and B = As, Sb, Si-C and for the Al-Ti system. For the Al-rich part of the Al-Ti system, also a semi-schematic non-equilibrium ES diagram is constructed. Based on these diagrams, the synthesis conditions of various phases has been discussed.

  19. The Use of Umbelliferone in the Synthesis of New Heterocyclic Compounds

    Directory of Open Access Journals (Sweden)

    Abu Bakar Mohamad

    2011-08-01

    Full Text Available New coumarin derivatives, namely 7-[(5-amino-1,3,4-thiadiazol-2-ylmethoxy]-2H-chromen-2-one (4, 5-[(2-oxo-2H-chromen-7-yloxymethyl]-1,3,4-thiadiazol-2(3H-one (5, 2-[2-(2-oxo-2H-chromen-7-yloxyacetyl]-N-phenylhydrazinecarbothioamide (7, 7-[(5-(phenylamino-1,3,4-thiadiazol-2-ylmethoxy]-2H-chromen-2-one (8 and 7-[(5-mercapto-4-phenyl-4H-1,2,4-triazol-3-ylmethoxy]-2H-chromen-2-one (9 were prepared starting from the natural compound umbelliferone (1. The newly synthesized compounds were characterized by elemental analysis and spectral studies (IR, 1H-NMR and 13C-NMR.

  20. Synthesis of hydantoin and thiohydantoin related compounds from benzil and study of their cytotoxicity

    Directory of Open Access Journals (Sweden)

    A. Kashem Liton and M. Rabiul Islam

    2006-06-01

    Full Text Available Condensation of benzil (1 with urea, monophenyl urea and diphenyl urea in the presence of absolute ethanol using 30% aqueous NaOH gave the products 1a, 1b and 1c respectively and also with thiourea, monomethyl thiourea, dimethyl thiourea and diethyl thiourea the products 2a, 2b, 2c and 2d were obtained. Methylation of the product, 2a in the presence of dimethyl formamide (DMF using K2CO3 formed 2. The compounds 1b, 1c, 2b, 2c and 2 showed highly cytotoxic activity and the compounds 1a, 2a, 2d showed relatively low cytotoxic activity against brine shrimp lethality bioassay.

  1. Chemoenzymatic synthesis of organoselenium(IV) compounds and their evaluation as cysteine protease inhibitors

    Energy Technology Data Exchange (ETDEWEB)

    Piovan, Leandro; Andrade, Leandro H., E-mail: leandroh@iq.usp.b [Universidade de Sao Paulo (USP), SP (Brazil). Inst. de Quimica; Alves, Marcio F.M.; Juliano, Luiz; Cunha, Rodrigo L.O.R, E-mail: rodrigo.cunha@ufabc.edu.b [Universidade Federal de Sao Paulo (Unifesp/EPM), Sao Paulo, SP (Brazil). Dept. de Biofisica; Broemme, Dieter [University of British Columbia, Vancouver (Canada). Dept. of Dentistry

    2010-07-01

    A series of organoselenium dihalides (organoselenanes) was synthesized from organoselenides using a chemoenzymatic approach. The organoselenanes have variations in their stereochemistry and in the halogen atom bonded to the selenium atom. Because of the unique selenium-thiol chemistry displayed by several organoselenium compounds, the organoselenanes were evaluated as new potential inhibitors of cysteine proteases (cathepsins S and V). By the analysis of the second-order rate constants of the inhibition of cathepsin S and V, it was possible to conclude that organoselenanes inhibited the cathepsin S faster than cathepsin V. It was observed higher inhibitory potencies for the dibromo organoselenanes derivatives than the dichloro analogues. In addition, the present data suggest the use of hypervalent selenium compounds as novel motifs for cysteine proteases inhibitors. (author)

  2. New guаnidin-containing compounds with biocidal active: synthesis and prospects of study

    Directory of Open Access Journals (Sweden)

    Nadejda Kyznecova

    2014-04-01

    Full Text Available Synthesized a new complex compound-ditsitratoborat guanidinium studied its composition, structure , physical and chemical properties using IR spectroscopy , thermal , X-ray diffraction and elemental analysis , conductivity , quantum-chemical modeling . Proven biocidal activity against Escherichia coli, Staphylo-coccus aureus, yeasts bioassay methods . On the basis of silicate (clay and the Trans-Baikal Territory materials synthesized coordination compound obtained organic-inorganic composites in various ways (using mechanical activation and ultrasonic vibrations , studied its properties. The present invention extends the range of antiseptic preparations , the resulting composite is promising a wide range of applications due to their sorption properties and biocidal activity : qualitative improvement of natural , domestic, wastewater , swimming pools, reservoirs , soil objects .

  3. Synthesis, Mass Spectrometric Studies, and Biological Evaluation of 3,5-Dimethoxyhomophthalic Acid and Related Compounds

    Institute of Scientific and Technical Information of China (English)

    GHULAM Qadeer; NASIM Hasan-rama; FAN Zhi-jin

    2007-01-01

    3,5-Dimethoxyhomophthalic acid was synthesized in four steps from 3,5-dimethoxycinnamic acid via a series of reactions including cyclization of 3-(3' ,5'-dimethoxyphenyl) propionic acid to 5,7-dimethoxy-1-indanone and oxidative decomposition of methyl-2-hydroxy-2-[ 5,7-dimethyoxy-1-oxo-1H-inden-2 (3H) -ylidene ] acetate to 3,5-dimethoxyhomophthalic acid. The synthesized compounds were characterized by elemental analysis, IR, 1H NMR, and MS. The biological evaluation experiments of 3,5-dimthoxyhomophthalic acid and the related synthesized compounds were also carried out. Naturally occurring biologically active isocoumarins were prepared in a single step by the condensation of the homophthalic acid with appropriate acid chlorides.

  4. Synthesis and Crystal Structure of Compound [ZnS6 (C12H8N2)

    Institute of Scientific and Technical Information of China (English)

    陈之荣; 李健晖; 李鸿钧; 苏卫平; 曹荣

    2000-01-01

    The title compound ZnS6(C12H8N2) was obtained by reaction of zinic powder with sulfur and 1,10-phenathtroline in DMF solvent, and its structure has been determined by single crystal X-ray diffraction analysis. The crystal data for the compound: triclinic, P-1, Z = 2, a = 8. 159(2), b = 9. 485(2), c = 11. 997(2)A , α =110. 00(3)°,β = 99.22(3)°, γ = 100.57(3)°, V = 832A3, Dc =1. 748g/cm3, μ(MoKa)=0. 2219 cm-1, F(000)=440. The structure was refined to R = 0. 0723 and Rw = 0. 0865 for 1427 independent observed reflections. The tilte crystal consists of a discrete molecules, in which the core of ZnS2N2 shows a distorted tetrahedral geometry.

  5. Synthesis and Broad-Spectrum Antiviral Activity of Some Novel Benzo-Heterocyclic Amine Compounds

    Directory of Open Access Journals (Sweden)

    Da-Jun Zhang

    2014-01-01

    Full Text Available A series of novel unsaturated five-membered benzo-heterocyclic amine derivatives were synthesized and assayed to determine their in vitro broad-spectrum antiviral activities. The biological results showed that most of our synthesized compounds exhibited potent broad-spectrum antiviral activity. Notably, compounds 3f (IC50 = 3.21–5.06 μM and 3g (IC50 = 0.71–34.87 μM showed potent activity towards both RNA viruses (influenza A, HCV and Cox B3 virus and a DNA virus (HBV at low micromolar concentrations. An SAR study showed that electron-withdrawing substituents located on the aromatic or heteroaromatic ring favored antiviral activity towards RNA viruses.

  6. Molecular modeling and synthesis of certain substituted aryl compounds which have a potential anticancer activity

    Directory of Open Access Journals (Sweden)

    Hosam A. Ahmed

    2011-06-01

    Conclusion: The results of this study had led to the identification of two lead compounds with good inhibitory activities that could overlay for the next generation of the inhibitors for methionine synthase. Preparation of novel potential inhibitors for the methionine synthase that have the ability to avoid the side effects of the other marketed anticancer drugs could be a good step forward towards cancer treatment.

  7. Synthesis and Characterisation of a Novel Phosphonate Ligand and Its Palladium(II Coordination Compound

    Directory of Open Access Journals (Sweden)

    Olesea Cuzan

    2017-06-01

    Full Text Available The novel N-(methylene-2-pyridine-N,N-bis(diethoxyphosphorylmethylamine ligand (L was obtained through a double Kabachnik-Fields reaction, starting from 2-aminomethyl pyridine (2-picolylamine. Based on the L ligand, a new palladium(II coordination compound [Pd(L2Cl2] has been synthetized and comprehensively characterized by spectroscopic methods (1H NMR, UV-Vis, ESI mass spectrometry and X-ray crystallography.

  8. a -Oxo Ketene Dithioacetals Chemistry-A Facile Route to the Synthesis of Fused Heterocyclic Compounds

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The fused heterocyclic compounds 2 : imidazo [1,2-a] pyridine 2a-c and pyrido [1,2-a] pyrimidine 2d were obtained from the reaction of a -cinnamoyl ketene dibenzylthio acetals 1 with diamine. When a -cinnamoyl -a '-benzoyl ketene N, N-acetals 3a-b were treated by t-BuONa/t-BuOH solution, 8- benzoyl-pyrido[1,2-a] pyrimidine 4 was produced.

  9. Studies on the Synthesis and the Structure of Ferric Aluminum Magnesium Hydrotalcite-like Compounds

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The particles of ferric aluminum magnesium hydrotalcite-like compounds (Fe-Al-Mg_HTlc) were synthesized by co-precipitation method. It was found that when n(Fe)/n(Al+Mg+Fe)0.30, Al(OH)3 will emerge; when the molar ratio of Fe/(Fe+Al+Mg) >0.30, the amorphous composition will appear. Hence Fe3+ and Al3+ have no concentration superposition effect on the crystal structure of the samples.

  10. SYNTHESIS, CRYSTAL STRUCTURE, SPECTROSCOPY PROPERTIES AND POTENTIAL ANTIMICROBIAL POTENTIALITIES OF A NEW SYNTHETIC COMPOUND: AMINO- CHLOROPYRIDINIUM DIAQUA DIOXALATO IRON(III

    Directory of Open Access Journals (Sweden)

    Jawher Abdelhak

    2014-12-01

    Full Text Available We report herein the synthesis and the physicochemical characterization of a new mixed-ligand iron(III complex of formula (C5H6ClN2[Fe(C2O42(H2O2].2H2O. This compound has been prepared by slow evaporation at room temperature and characterized by single crystal X-ray diffraction. It has been characterized by IR and UV-VIS spectra and thermal analysis (TG and DTA. In this compound, the iron ion has a slightly distorted square bipyramidal environment, coordinated by two chelating oxalate ion and two water molecules. Structural cohesion is established essentially by π-π interactions between the rings of pyridine groups and intermolecular hydrogen bonds connecting the ionic entities and uncoordinated water molecules. In vitro antimicrobial activities of the amino- chloropyridinium diaqua dioxalato iron (III against pathogenic fungi, yeast and bacteria were studied in this work. On the whole, our new compound has high antibacterial activities against Pseudomonas aeruginosa, Staphylococcus aureus and Listeria innocua. The amino- chloropyridinium diaqua dioxalato iron (III used at 200µg m-1, can reduce Candida albicans survival of about 45.45%, and destruct hyphe mycelial of Trichophyton rubrum. High lysozyme activities were expressed especially against Listeria innocua with 17 times more than Staphylococcus aureus. The minimal inhibitory concentrations (MIC are ranging from 16 µg ml-1 for bacteria to 256 µg ml-1 for yeast and IC50 values varying from 1.44 to 10.45 µg ml-1 for bacteria and 45.8 for yeast.

  11. Synthesis, Crystal and Electronic Structure of the Quaternary Magnetic EuTAl4Si2 (T = Rh and Ir) Compounds

    Energy Technology Data Exchange (ETDEWEB)

    Maurya, Arvind [Tata Institute of Fundamental Research; Thamizhavel, Arumugam [Tata Institute of Fundamental Research; Provino, Alessia [University of Genova; Pani, Marcella [University of Genova; Manfrinetti, Pietro [University of Genova; Paudyal, Durga [Ames Laboratory; Dhar, Sudesh Kumar [Tata Institute of Fundamental Research

    2014-01-22

    Single crystals of the quaternary europium compounds EuRhAl4Si2 and EuIrAl4Si2 were synthesized by using the Al–Si binary eutectic as a flux. The structure of the two quaternary compounds has been refined by single crystal X-ray diffraction. Both compounds are stoichiometric and adopt an ordered derivative of the ternary KCu4S3 structure type (tetragonal tP8, P4/mmm). The two compounds reported here represent the first example of a quaternary and truly stoichiometric 1:1:4:2 phase crystallizing with this structure type. In light of our present results, the structure of the BaMg4Si3 compound given in literature as representing a new prototype is actually isotypic with the KCu4S3 structure. Local spin density approximation including the Hubbard U parameter (LSDA + U) calculations show that Eu ions are in the divalent state, with a significant hybridization between the Eu 5d, Rh (Ir) 4d (5d), Si 3p and Al 3p states. Magnetic susceptibility measured along the [001] direction confirms the divalent nature of the Eu ions in EuRhAl4Si2 and EuIrAl4Si2, which order magnetically near 11 and 15 K, respectively.

  12. In Situ Synthesis of Nanocrystalline Intermetallic Compound Layer during Surface Mechanical Attrition Treatment of Zirconium

    Institute of Scientific and Technical Information of China (English)

    SUNCai-yun; XIEJi-jia; WUXiao-lei; HONGYou-shi; LIUGang; LUJian; LUKe

    2004-01-01

    The surface mechanical attrition treatment (SMAT) technique was developed to synthesize a nanocrystalline (NC) layer on the surface of metallic materials for upgrading their overall properties and performance. In this paper, by means of SMAT to a pure zirconium plate at the room temperature, repetitive multidirectional peening of steel shots (composition (wt%): 1C, 1.5Cr, base Fe) severely deformed the surface layer. A NC surface layer consisting of the intermetallic compound FeCr was fabricated on the surface of the zirconium. The microstructure characterization of the surface layer was performed by using X-ray diffraction analysis, optical microscopy, scanning and transmission electron microscopy observations. The NC surface layer was about 25μm thick and consisted of the intermetallic compound FeCr with an average grain size of 25+10 nm. The deformation-induced fast diffusion of Fe and Cr from the steel shots into Zr occurred during SMAT, leading to the formation of intermetallic compound. In addition, the NC surface layer exhibited an ultrahigh nanohardness of 10.2 GPa.

  13. Synthesis, algal inhibition activities and QSAR studies of novel gramine compounds containing ester functional groups

    Institute of Scientific and Technical Information of China (English)

    LI Xia; YU Liangmin; JIANG Xiaohui; XIA Shuwei; ZHAO Haizhou

    2009-01-01

    2,5,6-Tribromo-l-methylgramine (TBG), isolated from bryozoan Zoobotryon pellucidum was shown to be very efficient in preventing recruitment of larval settlement. In order to improve the compatibility of TBG and its analogues with other ingredients in antifouling paints, structural modification of TBG was focused mainly on halogen substitution and N-substitution. Two halogen-substitute gramines and their derivatives which contain ester functional groups at N-position of gramines were synthesized. Algal inhibition activities of the synthesized compounds against algae Nitzschia closterium were evaluated and the Median Effective Concentration (EC50) range was 1.06-6.74 μg ml-1. Compounds that had a long chain ester group exhibited extremely high antifouling activity. Quantitive Structure Activity Relationship (QSAR) studies with multiple linear regression analysis were applied to find correlation between different calculated molecular descriptors and biological activity of the synthesized compounds. The results show that the toxicity (log (1/EC50)) is correlated well with the partition coefficient log P. Thus, these products have potential function as antifouling agents.

  14. Synthesis of Hydroxide-TiO2 Compounds with Photocatalytic Activity for Degradation of Phenol

    Science.gov (United States)

    Contreras-Ruiz, J. C.; Martínez-Gallegos, S.; Ordoñez, E.; González-Juárez, J. C.; García-Rivas, J. L.

    2017-03-01

    Photocatalytic degradation of phenol using titanium dioxide (TiO2), either alone or in combination with other materials, has been tested. Mg/Al hydrotalcites prepared by two methods using inorganic (HC) or organic (HS) chemical reagents, along with mixed oxides produced by calcination of these products (HCC and HSC), were mixed with titanium isopropoxide to obtain hydroxide-TiO2 compounds (HCC-TiO2 and HSC-TiO2) and their photocatalytic activity tested in solutions of 10 mg/L phenol at 120 min under illumination at λ UV = 254 nm with power of 4 W or 8 W. The obtained materials were characterized by various techniques, revealing that TiO2 was incorporated into the mixed oxides of the calcined hydrotalcite to form the above-mentioned compounds. The photocatalytic test results indicate that the activity of HCC-TiO2 can be attributed to increased phenol adsorption by hydrotalcite for transfer to the active photocatalytic phase of the impregnated TiO2 particles, while the better results obtained for HSC-TiO2 are due to greater catalyst impregnation on the surface of the calcined hydrotalcite, reducing the screening phenomenon and achieving HSC-TiO2 degradation of up to 21.0% at 8 W. Reuse of both compounds indicated tight combination of HCC or HSC with TiO2, since in four successive separation cycles there was little reduction of activity, being associated primarily with material loss during recovery.

  15. Synthesis, Structure and Biological Activities of Novel Triazole Compounds Containing Thioamide Group

    Institute of Scientific and Technical Information of China (English)

    刘法谦; 秦永其; 许良忠; 陆路德; 杨绪杰; 汪信

    2005-01-01

    Two compounds 2-benzoyl-N-phenyl-2-( 1,2,4-triazol- 1-yl)thioacetamide (1) and 2-(4-chlorobenzoyl)-N-phenyl-2-(1,2,4-triazol-1-yl)thioacetamide (2) were synthesized from substituted acetophenone, triazole and phenyl isothiocyanate by several step reactions. The structure of compound 1 was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic system with space group P21/c, a =0.8806(2) nm, b= 1.2097(2) nm, c= 1.4809(3) nm, β=105.88°, Z=4, V=1.5173(6) nm3, Dc= 1.411 Mg/m3, μ=0.22 mm-1, F(000)=672, final R1=0.040 and Rw=0.103. There is obvious potentially weak C—H…N intermolecular interaction in the crystal, which stabilizes the structure. The results of biological test show that the two compounds have antifungal and plant growth regulating activities.

  16. DBU-catalyzed, aromatization-oriented, regioselective domino synthesis of 2-aminopyrimidines from [Formula: see text]-dicarbonyl compounds, DMF-DMA, and cyanamide.

    Science.gov (United States)

    Üngören, Şevket Hakan; Boz, Şerife

    2017-08-01

    A multicomponent domino synthesis has been developed for the preparation of 2-aminopyrimidines from [Formula: see text]-dicarbonyl compounds, N,N-dimethylformamide dimethyl acetal, and cyanamide. The protocol was used for the regioselective preparation of 4-amide/ester/ketone substituted 2-aminopyrimidines. Twelve 2-aminopyrimidines were isolated in good yields (56-93%).

  17. NEW SHEET MOLDING COMPOUND RESINS FROM SOYBEAN OIL. I. SYNTHESIS AND CHARACTERIZATION. (R829576)

    Science.gov (United States)

    The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

  18. Rapid Synthesis of Flavor Compound 4-Ethyloctanoic Acid under Microwave Irradiation

    Science.gov (United States)

    Liu, Yu-Ping; Yin, De-Cai; Chen, Hai-Tao; Sun, Bao-Guo

    2010-01-01

    Rapid synthesis of 4-ethyloctanoic acid by means of microwave irradiation is described. Diethyl malonate reacted with 2-ethyl-1-bromohexane in the presence of sodium ethoxide to give diethyl (2-ethylhexyl)malonate (1b). 1b was saponified in the solution of ethanol and potassium hydroxide and then acidified to form (2-ethylhexyl)propanedioic acid (1c), and 1c was heated and decarboxylized to give 4-ethyloctanoic acid (1d). The influence of reaction temperature and reaction time on the yield of 1b and the effect of reaction time on the yield of 1c and 1d were investigated in order to optimize the synthetic conditions. The relative optimal conditions for the synthesis of 1b were a mole ratio of sodium to diethyl malonate to 2-ethylhexyl bromide of 0.1:0.11:0.11, a reaction temperature of 80–85 °C, and a reaction time of 2–2.5 h. The yield of 1b was about 79%. 1b was saponified for 30 min and then acidified to form 1c, and the yield of 1c was 96%. 1c was heated for 16 min at 180°C to give 1d, and the yield of 1d was about 90%. The overall yield of 1d is 70% under microwave irradiation. The reaction time was reduced greatly. In order to compare the result of microwave irradiation with that of an oil bath, the reactions were also performed in an oil bath. The structures of intermediates, product and by-product were confirmed by HRMS, 1H NMR, 13C-NMR and IR. PMID:21152328

  19. Data collection from energy certificates. Experiences and analysis. Synthesis report

    Energy Technology Data Exchange (ETDEWEB)

    Loga, Tobias; Diefenbach, Nikolaus (eds.); Popiolek, Malgorzata; Panek, Aleksander [Narodowa Agencja Poszanowania Energii S.A. (NAPE), Warsaw (Poland); Cohen, Robert [Energy for Sustainable Development Ltd (ESD), Overmoor (GB)] (and others)

    2008-03-15

    Apart from the described bottom-up approach DATAMINE also aims at drawing general conclu-sions concerning monitoring with the help of energy certificates. Of course 12 projects simultane-ously being carried out in 12 EU countries bring up the question if there is a way for a common analysis of the collected data or at least for a common understanding of the data from different projects. Against that background a harmonised data structure with 255 data fields was defined. The ''philosophy'' of this approach was as follows: Each project partner could use his own data structure and carry out his analysis in an individual way according to the objectives and conditions of his individual model project. But at the end he had to translate his data base in the harmonised data structure and to deliver it to the project coordinator IWU who collect all data in a common evaluation data base. This will make possible a cross-country comparison of the collected data - taking into consideration that because of the different types of energy certificates neither all data fields of the data structure can be filled in by the model projects nor will a comparison of all model projects be possible. So the harmonised data structure can be seen as a simplified ''common lan-guage'' that facilitates an understanding of data bases from different projects. A detailed descrip-tion of the data structure among with other general results from the first DATAMINE workpackages which were carried out before the model projects is given in the DATAMINE synthesis report ''Con-cepts for Data Collection and Analysis'' from December 2006 which is also available on the project website. (orig.)

  20. General synthesis of carbon nanocages and their adsorption of toxic compounds from cigarette smoke

    Science.gov (United States)

    Li, Guangda; Yu, Hongxiao; Xu, Liqiang; Ma, Qiang; Chen, Chao; Hao, Qin; Qian, Yitai

    2011-08-01

    Carbon nanocages (CNCs) have been synthesized through a simple approach using different alcohols and ferrous oxalate as reactants at 550 °C for 12 h in a sealed autoclave. The lengths of the sides of the CNCs are about 200-350 nm and the wall thicknesses are about 10-15 nm. The formation mechanism of the CNCs is also discussed, based on the experimental results. These CNCs show excellent removal efficiency for phenolic compounds, ammonia, and total particulate matter from cigarette smoke. The adsorption capability of CNCs prepared from ethanol is much higher than that of other samples. For example, the efficiency of 5 mg CNCs (ethanol) for removing the six phenolic compounds p-dihydroxybenzene, m-dihydroxybenzene, o-dihydroxybenzene, phenol, m-cresol, and o-cresol can reach 57.31%, 62.25%, 65.58%, 75.95%, 54.34% and 59.43%, respectively, while that of the commercial activated carbon (5 mg) can only reach 29.02%, 33.93%, 35.00%, 36.00%, 20.33% and 36.19%, respectively, under the same conditions.Carbon nanocages (CNCs) have been synthesized through a simple approach using different alcohols and ferrous oxalate as reactants at 550 °C for 12 h in a sealed autoclave. The lengths of the sides of the CNCs are about 200-350 nm and the wall thicknesses are about 10-15 nm. The formation mechanism of the CNCs is also discussed, based on the experimental results. These CNCs show excellent removal efficiency for phenolic compounds, ammonia, and total particulate matter from cigarette smoke. The adsorption capability of CNCs prepared from ethanol is much higher than that of other samples. For example, the efficiency of 5 mg CNCs (ethanol) for removing the six phenolic compounds p-dihydroxybenzene, m-dihydroxybenzene, o-dihydroxybenzene, phenol, m-cresol, and o-cresol can reach 57.31%, 62.25%, 65.58%, 75.95%, 54.34% and 59.43%, respectively, while that of the commercial activated carbon (5 mg) can only reach 29.02%, 33.93%, 35.00%, 36.00%, 20.33% and 36.19%, respectively, under

  1. Synthesis of Hydrotalcite-like Compound Pillared by Hetero-polyacid Anions in a Hydrothermal System

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Hetero-polyacid anions (PW12O403-)-pillared hydrotalcite-like compound is directly and hydrothermally synthesized by the hot solution method. FTIR and XRD show that PW12O403- has been incorporated into the interstitial space with the dimension of 0.917 nm. The state of PW12O403- anion between the hydrotalcite sheets was also discussed. The title product can be expressed by formula [Zn0.68Al0.32(OH)2][PW12O40] 0. 113H2O after a serious study of TGA and chemical analysis.

  2. Synthesis and structural analysis of a regular Cu-Mg-Al hydrotalcite-like compound

    OpenAIRE

    WU, Jian-Song; XIAO, Ying-Kai; Liu, Yu-ping; XU, Wan-Bang

    2011-01-01

    A fine-quality, regular Cu-Mg-Al hydrotalcite-like compound was synthesized via the glycothermal method using CuCl2 \\cdot 2H2O, MgCl2 \\cdot 6H2O, AlCl3 \\cdot 6H2O, and Na2CO3 as raw materials and sodium hydroxide as the precipitant. Hydrotalcite samples were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric-differential thermal analysis, and Brunauer-Emmett-Teller N2 surface ar...

  3. Synthesis and Characterization of a Novel Compound SnDy2O4

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A new phase, the rare earth complex oxide SnDy2O4 was synthesized by the thermal decomposition of its oxalate precursor that was prepared by rheological phase reaction method. TG, IR, XRD and EPS were used to prove the formation of the compound SnDy2O4. The structure of SnDy2O4 was refined by Rietveld analysis. SnDy2O4 is cubic, a = 7.40366A, V = 405.82A3, Z = 4.

  4. A green synthesis of α,β-unsaturated carbonyl compounds from glyceraldehyde acetonide

    Directory of Open Access Journals (Sweden)

    Cláudia O. Veloso

    2011-01-01

    Full Text Available The catalytic behavior of Cs-exchanged and Cs-impregnated zeolites (X and Y was studied using the Knoevenagel condensation between glyceraldehyde acetonide and ethyl acetoacetate in order to produce the corresponding α,β-unsaturated carbonyl compound that is an important intermediate for fine chemicals. The influence of reaction temperature, type of zeolite, and basicity of the sites on the catalytic behavior of the samples was evaluated. All zeolites were active for the studied reaction. The formation of the main condensation product was favored at lower reaction temperatures. Products of further condensations were also observed especially for samples that were only dried before catalytic test.

  5. Synthesis and mesomorphic properties of novel [1,2,3]-triazole mesogenic based compounds

    Science.gov (United States)

    Benbayer, Chahinez; Kheddam, Narimane; Saïdi-Besbes, Salima; Givenchy, Elisabeth Taffin de; Guittard, Frédéric; Grelet, Eric; Safer, Abdel Mounaim; Derdour, Aïcha

    2013-02-01

    A series of five-membered heterocyclic 1,2,3-triazole derivatives with different substituents in N1 position was synthesized. The heterocyclic moiety was connected through an ester function to a p-decyloxyphenyl or p-decyloxybiphenyl tails Polarized microscopy studies, X-ray scattering and differential scanning calorimetry (DSC) analysis revealed that the target compounds exhibit enantiotropic liquid crystalline properties. Their mesomorphic behavior is closely related to the nature of the substituent X present in N1 position of the heterocycle.

  6. SYNTHESIS AND CRYSTAL STRUCTURE OF A NEW COMPOUND Sr6Sn2Nb8O30

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    A new compound Sr6Sn2Nb8O30 was found in th e ternary system of SrO-SnO2-Nb2O5.The transparent colorless crystal wit h n eedle-like shape can be grown by flux method.The crystal structure of new compo un d was determined by X-ray diffraction, and its belongs to tungsten bronze struc ture.Sr6Sn2Nb8O30 crystallizes in orthorhombic system with unit cell parameters a=17.579(1),b=17.509(1),c=7.7880(5),Z=4 and space group Cmm2.

  7. Synthesis, Mechanism of Formation and Insecticidal Activity of Novel Fluorinated Organophosphorus Compounds

    Institute of Scientific and Technical Information of China (English)

    WU,Jun(吴军); HUDSON,Harry R.

    2002-01-01

    The major products of the interaction between triethyl phosphite and 3-fluoropropanoyl chloride at room temperamre are diethyl ( E )-1-( 3-fluoropropanoyioxy )-3-fluoroprop-1-enylphosphonate (3) and diethyl 1-( diethoxyphosphoryl)-3-fluoropropyl phosphate (4). The compounds 3 and 4 were separated by chromatography, and structurally characterized by elemental analysis, NMR spectroscopy (1H, 13C, 19F and 31p) and mass spectrometry. Possible reaction mechanisms are proposed. The major products 3 and 4 were tested for insecticidal activity. 3 gave 100% control of Musca domestica L. and Phaedon cochledriae Fab. at a dose of 20 μg/per insect.

  8. Group IV Mixed Sandwich Compounds : Synthesis of Pentamethylcyclopentadienyl-Titanium, -Zirconium and -Hafnium Cycloheptatrienyl and Cyclooctatetraene Complexes

    NARCIS (Netherlands)

    Blenkers, J.; Bruin, P.; Teuben, J.H.

    1985-01-01

    The first complete series of Group IV sandwich complexes Cp*MCHT (M = Ti, Zr, Hf) (Cp* = η5-C5Me5, CHT = η7-C7H7) has been made and characterized. Cp*HfCHT is the first reported sandwich compound of hafnium. The d1, η8-C8H8(COT) complex Cp*MCOT were also synthesised similarly for M = Ti, Zr, but the

  9. Development of Ni-Based Catalysts Derived from Hydrotalcite-Like Compounds Precursors for Synthesis Gas Production via Methane or Ethanol Reforming

    Directory of Open Access Journals (Sweden)

    Ya-Li Du

    2017-02-01

    Full Text Available As a favorably clean fuel, syngas (synthesis gas production has been the focus of concern in past decades. Substantial literatures reported the syngas production by various catalytic reforming reactions particularly in methane or ethanol reforming. Among the developed catalysts in these reforming processes, Ni-based catalysts from hydrotalcite-like compounds (HTLcs precursors have drawn considerable attention for their preferable structural traits. This review covers the recent literature reporting syngas production with Ni-based catalysts from HTLc precursors via methane or ethanol reforming. The discussion was initiated with catalyst preparation (including conventional and novel means, followed by subsequent thermal treatment processes, then composition design and the addition of promoters in these catalysts. As Ni-based catalysts have thermodynamic potential to deactivate because of carbon deposition or metal sintering, measures for dealing with these problems were finally summarized. To obtain optimal catalytic performances and resultantly better syngas production, based on analyzing the achievements of the references, some perspectives were finally proposed.

  10. Single-Bead Quantification of Peptide Loading Distribution for One-Bead One-Compound Library Synthesis Using Confocal Raman Spectroscopy.

    Science.gov (United States)

    Tang, Yuchen; Thillier, Yann; Liu, Ruiwu; Li, Xiaocen; Lam, Kit S; Gao, Tingjuan

    2017-07-05

    We report an analytical method to determine peptide loading of "one-bead one-compound" (OBOC) combinatorial peptide libraries at single-bead level. The quantification is based on a linear relationship between the amount of N-terminal amino groups on individual peptide beads and the intensity of Raman signal obtained from a specifically designed reporter labeled on amino groups. Confocal Raman spectroscopy was employed to characterize peptide loading of beads with defined peptide sequences and from OBOC combinatorial peptide libraries. Although amine loading of blank TentaGel beads was found to be uniform, peptide loading among beads of OBOC peptide libraries varied substantially, particularly for those libraries with long sequences. Construction of OBOC libraries can be monitored with this novel analytical technique so that synthetic conditions can be optimized for the preparation of high-quality OBOC peptide libraries. As the variability of peptide loading of individual library beads can significantly influence the screening results, quantitative information obtained by this method will allow us to gain insight into the complexity and challenge of OBOC library synthesis and screening.

  11. Synthesis and chemistry of organoimidovanadium(V) compounds and their role in the formation of vanadium nitrides

    Science.gov (United States)

    Gipson, Rocky Dean

    A series of vanadium(V) compounds of the formula (eta5-C 5Me5)V(NR)Cl2 (R = 1-adamantyl, tert-butyl, para-tolyl) have been prepared by the reaction of (eta5 -C5Me5)V(O)Cl2 with RNCO or by oxidation of [(eta5-C5Me5)VCl2] 3 with azide. The para-tolylimido compound undergoes chloride metathesis with monoanionic reagents NaOtBu, LiNEt 2, and Mg(CH2SiMe3)2 to produce mono- and disubstituted products. A discussion of ligand strength in this system using 51V NMR is presented. Ammonolysis of the dichloro compounds produces the symmetrically-bridged [(eta5-C5Me5)V(mu-N)Cl]2, in yields consistent with the basicity of the organoimido ligand. A comparison of this reactivity with that of (eta5-C5Me 5)V(NSiMe3)Cl2 is presented. An X-ray structural study of (eta5-C5Me5)V(NtBu)Cl 2 exhibits a 173° V-N-C imido linkage and V-N triple bond. Synthesis of (eta5-tBuC5H 4)V(NR)Cl2 compounds was performed utilizing (t-Bu)C 5H4SiMe3 as the cyclopentadiene reagent with V(NR)Cl 3. In contrast to the metathesis of V(NR)Cl3 compounds with Li(tBu)C5H4, reduction of the vanadium(V) is not observed. An X-ray crystal structure of (eta5- tBuC5H4)V(N-ptol)Cl2 reveals linear V-N-C bonding, and a short N-C bond of 139 pm. This is explained by delocalized bonding, which incorporates the imido carbon atoms as well as nitrogen and vanadium. Details of the structure and valence-bond descriptions are of this compound are presented. Organoimidotrichlorovanadium(V) compounds bind ligands L2 (L2 = 1,2-dimethoxyethane; N,N,N,N-tetramethylethylenediamine) to produce adducts V(NR)Cl3L2. The V(NR)Cl3L 2 compounds thermally react to form terminal nitrides V(N)Cl2L 2 via an unprecedented cleavage of the N-C bond of the organoimido ligand, with reactivity following the order t-butyl > 1-adamantyl > p-tolyl. The downfield 51V NMR shifts of the adducts relative to starting materials is discussed using crystal-field models. X-ray crystal structures of V(NAd)Cl3(DME) and V(N ptol)Cl3(TMEDA) are presented, and details

  12. Ectopic Compound Odontoma in the Buccal Mucosa: Report of a Rare Case

    Directory of Open Access Journals (Sweden)

    Aparna Venigalla

    2015-01-01

    Full Text Available Eruption of tooth into extraosseous locations is an extremely rare condition. We report a case of a six-year-old girl child with tooth-like structure erupting from the right buccal mucosa. Clinical, radiographic, and histopathologic examination suggested the diagnosis of compound odontoma. Very few cases have been reported so far, where tooth has been located completely in the soft tissue and a variety of names have been used for that condition. A brief review of the literature and the ambiguity in naming the situation is discussed.

  13. Ectopic compound odontoma in the buccal mucosa: report of a rare case.

    Science.gov (United States)

    Venigalla, Aparna; Guttikonda, Leela Krishna; Nelakurthi, Hasini; Babburi, Suresh; Pinisetti, Soujanya; Kotti, Ajay Banerji; Kalapala, Lavanya

    2015-01-01

    Eruption of tooth into extraosseous locations is an extremely rare condition. We report a case of a six-year-old girl child with tooth-like structure erupting from the right buccal mucosa. Clinical, radiographic, and histopathologic examination suggested the diagnosis of compound odontoma. Very few cases have been reported so far, where tooth has been located completely in the soft tissue and a variety of names have been used for that condition. A brief review of the literature and the ambiguity in naming the situation is discussed.

  14. Synthesis and fluorescence properties of six fluorescein-nitroxide radical hybrid-compounds.

    Science.gov (United States)

    Sato, Shingo; Endo, Susumu; Kurokawa, Yusuke; Yamaguchi, Masaki; Nagai, Akio; Ito, Tomohiro; Ogata, Tateaki

    2016-12-05

    Six fluorescein-nitroxide radical hybrid-compounds (2ab, 3ab, 4, and 5) were synthesized by the condensation of 5- or 6-carboxy-fluorescein and 4-amino-TEMPO (2ab), 5- or 6-aminofluorescein and 4-carboxy-TEMPO (3ab), and fluorescein and 4-carboxy-TEMPO (4), or by reaction of the 3-hydroxyl group of fluorescein with DPROXYL-3-ylmethyl methanesulfonate (5). Fluorescence intensities (around 520nm) after reduction of the radical increased to 1.43-, 1.38-, and 1.61-folds for 2a, 2b and 3b respectively; 3a alone exhibited a decrease in intensity on reduction. Since 4 was readily solvolyzed in PBS or even methanol to afford fluorescein and 4-carboxy-TEMPO, its fluorescence change could not be measured. Hybrid compound 5 containing an ether-linkage between the fluorescein phenol and 3-hydroxymethyl-DPROXYL hydroxyl centers, was stable and on reduction, showed a maximum increase (3.21-fold) in relative fluorescence intensity in PBS (pH5.0), despite its remarkably low absolute fluorescence intensity.

  15. Synthesis and Biological Activity of 2-Methylene Analogues of Calcitriol and Related Compounds.

    Science.gov (United States)

    Sibilska, Izabela K; Szybinski, Marcin; Sicinski, Rafal R; Plum, Lori A; DeLuca, Hector F

    2015-12-24

    In an attempt to prepare vitamin D analogues that are superagonists, (20R)- and (20S)-isomers of 1α-hydroxy-2-methylenevitamin D3 and 1α,25-dihydroxy-2-methylenevitamin D3 have been synthesized. To prepare the desired A-ring dienyne fragment, two different approaches were used, both starting from the (-)-quinic acid. The obtained derivative was subsequently coupled with the C,D-ring enol triflates derived from the corresponding Grundmann ketones, using the Sonogashira reaction. Moreover, (20R)- and (20S)-1α,25-dihydroxy-2-methylenevitamin D3 compounds with an (5E)-configuration were prepared by iodine catalyzed isomerization. All four 2-methylene analogues of the native hormone were characterized by high in vitro activity. As expected, the 25-desoxy analogues were much less potent. Among the synthesized compounds, two of them, 1α,25-dihydroxy-2-methylenevitamin D3 and its C-20 epimer, were found to be almost as active as 2-methylene-19-nor-(20S)-1α,25-dihydroxyvitamin D3 (2MD) on bone but more active in intestine.

  16. Organic compounds containing methoxy and cyanoacrylic acid: Synthesis, characterization, crystal structures, and theoretical studies

    Energy Technology Data Exchange (ETDEWEB)

    Khalaji, A. D., E-mail: alidkhalaji@yahoo.com [Golestan University, Department of Chemistry, Faculty of Science (Iran, Islamic Republic of); Maddahi, E. [Iran University of Science & Technology, Ms.C Educated, Department of Chemistry (Iran, Islamic Republic of); Dusek, M.; Fejfarova, K. [Institute of Physics of the ASCR, v.v.i. (Czech Republic); Chow, T. J. [Academia Sinica, Institute of Chemistry (China)

    2015-12-15

    Metal-free organic compounds 24-SC ((E)-2-cyano-3-(2,4-dimethoxyphenyl)acrylic acid) and 34-SC ((E)-2-cyano-3-(3,4-dimethoxyphenyl)acrylic acid), containing methoxy groups as a donor and the acrylic acid as an acceptor were synthesized and characterized by CHN, FT-IR, UV-Vis, {sup 1}H-NMR and single crystal X-ray diffraction and used as photosensitizers for the application of dye-sensitized solar cells (DSSC). The sensitizing characteristics of them were evaluated. Both compounds contain the natural molecule, its anionic form and the piperidinium cation and they differ by number of these molecules in the asymmetric unit. To get further insight into the effect of molecular structure on the performance of DSSC, their geometry and energies of HOMO and LUMO were optimized by density functional theory calculation at the B3LYP/6-31G(d) level with Gaussian 03. Overall conversion efficiencies of 0.78 under full sunlight irradiation are obtained for DSSCs based on the new metal-free organic dyes 24-SC and 34-SC.

  17. Two 8-Hydroxyquinolinate Based Supramolecular Coordination Compounds: Synthesis, Structures and Spectral Properties

    Directory of Open Access Journals (Sweden)

    Chengfeng Zhu

    2017-03-01

    Full Text Available Two new Cr(III complexes based on 2-substituted 8-hydroxyquinoline ligands, namely [Cr(L13] (1, (HL1=(E-2-[2-(4-nitro-phenyl-vinyl]-8-hydroxy-quinoline and [Cr(L23] (2, (HL2=(E-2-[2-(4-chloro-phenylvinyl]-8-hydroxy-quinoline, were prepared by a facile hydrothermal method and characterized thoroughly by single crystal X-ray diffraction, powder X-ray diffraction, FTIR, TGA, ESI-MS, UV-Visible absorption spectra and fluorescence emission spectra. Single crystal X-ray diffraction analyses showed that the two compounds featured 3D supramolecular architectures constructed from noncovalent interactions, such as π···π stacking, C-H···π, C-H···O, C-Cl···π, C-H···Cl interactions. The thermogravimetric analysis and ESI-MS study of compounds 1 and 2 suggested that the Cr(III complexes possessed good stability both in solid and solution. In addition, the ultraviolet and fluorescence response of the HL1 and HL2 shown marked changes upon their complexation with Cr(III ion, which indicated that the two 8-hydroxyquinolinate based ligand are promising heavy metal chelating agent for Cr3+.

  18. Synthesis, Structure and Biological Activities of Novel Triazole Compounds Containing N,N-Dialkyldithiocarbamate Moiety

    Institute of Scientific and Technical Information of China (English)

    XU,Liang-Zhong(许良忠); JIAN,Fang-Fang(建方方); SHI,Jian-Gang(时建刚); SUN,Ping-Ping(孙萍萍); JIAO,Kui(焦奎)

    2004-01-01

    The two compounds, 2,2-dimethyl-4-S-(N,N-dimethyldithiocarbamato)-5-(1,2,4-triazol-1-yl)-propione (1) and 2,2-dimethyl-4-S-(N,N-diethyldithiocarbamato)-5-(1,2,4-triazol-1-yl)-3-propione (2), were prepared by reacting N,N-dialkyldithiocarbamate sodium with 2,2-dimethyl-4-bromo-5-(1,2,4-triazol-1-yl)-propione. Their structures were identified by elemental analysis, IR and 1H NMR spectroscopy. The structure of 1 has been determined by X-ray single crystal structure analysis. It crystallizes in monoclinic system with space group P21/c, a= 1.2315(3)nm, b =1.2057(2) nm, c=1.2532(3) nm, β=118.55(3)° Z=4, V= 1.6345(6) nm3, Dc= 1.221 g/cm3, μ=0.324 mm -1, F(000)=640, final R1 =0.0449. There is obvious potentially weak C-H…N intermolecular interaction in the crystal, which stabilizes the crystal structure. The result of the biological test showed that the two compounds have fungistasis and plant growth regulating activities.

  19. Study on the Reaction of Benzimidazolium Salt with Amine Compounds

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    The addition-hydrolysis reaction of benzimidazolium salt with some mono- andbifunctional amine nucleophiles is reported, and a novel method of biomimetic synthesis forformamides and heterocycle compounds is provided.

  20. 8-(Dimethylamino)naphthylcopper(I), a novel stable organocopper compound with unusual structural features. A study concerning its synthesis, structure (X-ray) and reactivity. Its synthesis, crystal structure (X-ray) and reactivity

    NARCIS (Netherlands)

    Koten, G. van; Wehman, E.; Knotter, M.; Spelten, H.; Heijdenrijk, D.; Mak, A.N.S.; Stam, C.H.

    1987-01-01

    The synthesis and isolation of a hydrocarbon- and ether-insoluble organocopper compound containing the rigid 8-(dimethylamino)naphthyl group is described. An X-ray determination of its structure revealed a tetranuclear copper aggregate, in which the Cu atoms are arranged in a parallelogram (Cu...Cu

  1. Synthesis of N-substituted derivatives of 8,11-dimethyl-3,5-dioxo-4-azatricyclo[5.2.2.0(2,6)]undec-8-en-1-yl acetate and screening of cytotoxic activity of selected azatricycloundecane compounds.

    Science.gov (United States)

    Kossakowski, Jerzy; Kuran, Bozena

    2008-01-01

    This paper reports the synthesis of a number of aminoalkyl derivatives of 8,11-dimethyl-3,5-dioxo-4-azatricyclo[5.2.2.0(2,6)]undec-8-en-1-yl acetate and 1,11 -dimethyl-4-azatricyclo [5.2.2.0(2,6)]undecan-3,5,8-tri-one. Fourteen compounds were prepared and the in vitro cytotoxic activities were evaluated against human cancer cell lines originating from solid tumors in the National Cancer Institute, Bethesda, MD, USA.

  2. Hybrid microwave synthesis and characterization of the compounds in the Li-Ti-O system

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Li Hong; Dong, Cheng; Guo, Juan [National Laboratory for Superconductivity, Institute of Physics and Beijing National Laboratory for Condensed Matter Physics, Chinese Academy of Science, P.O. Box 603, Beijing 100080 (China)

    2008-01-03

    Hybrid microwave synthesis has been applied for preparation of Li{sub 4}Ti{sub 5}O{sub 12}, Li{sub 2}Ti{sub 3}O{sub 7}, Li{sub 2}TiO{sub 3} and LiTiO{sub 2} for the first time. Stepwise heating was used for avoiding the instantaneous release of gas by-product and obtaining well-shaped samples. The samples were characterized by powder X-ray diffraction, energy-dispersive X-ray analysis and scanning electron microscopy. The obtained samples have relatively uniform particle sizes. The electrochemical performance of Li{sub 4}Ti{sub 5}O{sub 12} and Li{sub 2}Ti{sub 3}O{sub 7} were investigated. The first discharge capacity of Li{sub 4}Ti{sub 5}O{sub 12} was 150 mAh g{sup -1} and 141 mAh g{sup -1} after 27 cycles and a very flat discharge and charge curve of Li{sub 4}Ti{sub 5}O{sub 12} was shown at about 1.56 V. Similarly, Li{sub 2}Ti{sub 3}O{sub 7} exhibits good cycle performance. The initial discharge capacity is 118 mAh g{sup -1} and 30th cycle is still 112 mAh g{sup -1}. (author)

  3. Synthesis of Phenolic Compounds by Trapping Arynes with a Hydroxy Surrogate

    Directory of Open Access Journals (Sweden)

    Rajdip Karmakar

    2015-08-01

    Full Text Available Trapping of arynes with various nucleophiles provides a range of heteroatom-functionalized arene derivatives, but the corresponding reaction with water does not provide phenol derivatives. Silver trifluroacetate (AgO2CCF3 can nicely solve this problem. It was found that in typical organic solvent, AgO2CCF3 readily reacts with arynes to generate trifluoroacetoxy organosilver arene intermediate, which, upon treating with silica gel, provides phenolic products. This protocol can be extended to the synthesis of α-halofunctionalized phenol derivatives by simply adding NBS (N-bromosuccinimides or NIS (N-iodosuccinimides to the reaction along with silver trifluroacetate, which provided α-bromo or α-iodophenol derivatives in good yield. However, the similar reactions with NCS (N-chlorosuccinimides afforded only the protonated product instead of the expected α-chlorophenols derivatives. Interestingly, substrates containing silyl substituents on 1,3-diynes resulted in α-halotrifluoroacetates rather than their hydrolyzed product. Additionally, trapping the same arynes with other oxygen-based nucleophiles containing silver counter cation, along with NXS (N-halosuccinimides, generated α-halooxyfunctionalized products.

  4. Hybrid microwave synthesis and characterization of the compounds in the Li-Ti-O system

    Science.gov (United States)

    Yang, Li Hong; Dong, Cheng; Guo, Juan

    Hybrid microwave synthesis has been applied for preparation of Li 4Ti 5O 12, Li 2Ti 3O 7, Li 2TiO 3 and LiTiO 2 for the first time. Stepwise heating was used for avoiding the instantaneous release of gas by-product and obtaining well-shaped samples. The samples were characterized by powder X-ray diffraction, energy-dispersive X-ray analysis and scanning electron microscopy. The obtained samples have relatively uniform particle sizes. The electrochemical performance of Li 4Ti 5O 12 and Li 2Ti 3O 7 were investigated. The first discharge capacity of Li 4Ti 5O 12 was 150 mAh g -1 and 141 mAh g -1 after 27 cycles and a very flat discharge and charge curve of Li 4Ti 5O 12 was shown at about 1.56 V. Similarly, Li 2Ti 3O 7 exhibits good cycle performance. The initial discharge capacity is 118 mAh g -1 and 30th cycle is still 112 mAh g -1.

  5. Design, synthesis, and biological properties of triazole derived compounds and their transition metal complexes.

    Science.gov (United States)

    Chohan, Zahid H; Hanif, Muhammad

    2010-10-01

    Triazole derived Schiff bases and their metal complexes (cobalt(II), copper(II), nickel(II), and zinc(II)) have been prepared and characterized using IR, (1)H and (13)C NMR, mass spectrometry, magnetic susceptibility and conductivity measurements, and CHN analysis data. The structure of L(2), N-[(5-methylthiophen-2-yl)methylidene]-1H-1,2,4-triazol-3-amine, has also been determined by the X-ray diffraction method. All the metal(II) complexes showed octahedral geometry except the copper(II) complexes, which showed distorted octahedral geometry. The triazole ligands and their metal complexes have been screened for their in vitro antibacterial, antifungal, and cytotoxic activity. All the synthesized compounds showed moderate to significant antibacterial activity against one or more bacterial strains. It is revealed that all the synthesized complexes showed better activity than the ligands, due to coordination.

  6. Synthesis of high refractive spiro heterocyclic derivatives through thioacetalization of multi-carbonyl compounds

    Energy Technology Data Exchange (ETDEWEB)

    Ye, Jim Young; Maheswara, Muchchintala; Do, Jung Yun [Pusan National Univ., Busan (Korea, Republic of)

    2012-04-15

    Preparation of several new spirocyclic mercaptol derivatives is described. Thiol protection on multi-carbonyl compounds allows of high sulfur content necessary to induce high refractive index. Condensation of 1,3-dimercapto-2-propanol and cyclohexanone followed by successive oxidation and thioacetalization affords a dispiro cycle with four sulfurs. Selective S,S-protection of cyclohexane-1,4-dione is achieved with 1,3-dimercapto-2-propanol and 2,3-dimercapto-1-propanol to provide dispiro cycles with four sulfurs. Olefineoxidation of norbornene gives a useful dialdehyde intermediate which is transformed to 1,3-dithiolane for a linearly-bound-cyclic molecule. Refractive index of linearly-bound-cycles was below 1.60 and dispiro cycles exhibited high refractive index of 1.57-1.69.

  7. Synthesis of Triazolone Compounds%三唑酮类化合物的合成

    Institute of Scientific and Technical Information of China (English)

    吴燕天; 黄龙江; 滕大为

    2015-01-01

    以4-哌啶甲酸为原料,经过缩合反应、酯化反应、关环反应(羰基亲核加成反应)、偶联反应合成目标产物三唑酮类化合物。研究了底物和反应条件(如配体、碱和溶剂)对偶联反应的影响。结果表明,以对甲氧基碘苯作底物、N , N-二甲基乙二胺作配体、CuI 作催化剂、K3 PO4作碱、N ,N-二甲基甲酰胺作溶剂时,三唑酮类化合物的产率达到最高,为60.3%。%Using 4-piperidine formic acid as raw material,the objective product triazolone compounds were synthesized by condensation reaction,esterification reaction,ring-closing reaction (carbonyl nucleophilic addi-tion reaction)and coupling reaction.The effects of reaction substrate and reaction conditions,such as ligand,al-kali,solvent on coupling reaction were studied.Results showed that the yield of triazolone compounds reached 60.3% when using methoxy iodobenzene as substrate,N ,N-dimethyl ethylenediamine as ligand,CuI as cata-lyst,K3 PO4 as alkali,N ,N-dimethyl formamide as solvent.

  8. Synthesis and evaluation of ?-hydroxy fatty acid-derived heterocyclic compounds with potential industrial interest

    Directory of Open Access Journals (Sweden)

    El-Sayed, R.

    2006-12-01

    Full Text Available T2-Hydroxyheptadecanoic acid chloride (2 reacted with anthranilic acid to produce 2-substituted-3,1-benzoxazin-4-one (3 which was used as starting material to synthesize some condensed and non-condensed heterocyclic compounds by reaction with nitrogen nucleophiles e.g., hydrazine hydrate, and formamide. The products were subjected to reaction with different moles of propylene oxide (n = 5, 10, 15 to produce a novel group of nonionic compounds having a double function as antibacterial and surface active agents which can be used in the manufacturing of drugs, cosmetics, pesticides or can be used as antibacterial and/or antifungal additives. The surface active properties as surface and interfacial tension, cloud point, foaming height, wetting time, and emulsification power were determined, the antimicrobial and biodegradability were also screened.El cloruro del ácido 2-hidroxiheptadecanoico (2 reaccionó con el ácido antranílico para producir 3,1-benzoxazin-4-onas 2-sustituidas que fueron usadas como material de partida en la síntesis de compuestos heterocíclicos condensados y no condensados por reacción con nucleófilos nitrogenados, como la hidracina o la formamida. Los productos fueron hechos reaccionar con diferentes moles de óxido de propileno (n = 5, 10, 15 para producir un grupo nuevo de compuestos no-iónicos teniendo una doble función como antibacterianos y tensoactivos que pueden ser usados en la manufactura de medicamentos, cosméticos, pesticidas, o pueden ser usados como aditivos antibacterianos y/o antifúngicos. Se determinaron diversas propiedades físicas de los compuestos preparados así como sus efectos antimicrobianos y sus biodegrabilidad.

  9. Synthesis and evaluation of ?-hydroxy fatty acid-derived heterocyclic compounds with potential industrial interest

    Directory of Open Access Journals (Sweden)

    El-Sayed, R.

    2007-03-01

    Full Text Available The reaction of 2-hydroxyheptadecanoyl chloride (2 and anthranilic acid gave 2-(1-hydroxyheptadecyl-4H-3,1-benzoxazin-4-one (3 which was used as starting material to synthesize some condensed and non-condensed heterocyclic compounds by a reaction with nitrogen nucleophiles (e.g., hydrazine hydrate, and formamide. The subsequent reaction of the synthetic products with different amounts of propylene oxide gave a novel group of nonionic compounds having a double function as antibacterial and surface active agents which may serve in the manufacturing of drugs, cosmetics, pesticides or as antibacterial and/or antifungal products. The surface active properties such as surface and interfacial tensions, cloud point, foaming height, wetting time, and emulsification power were determined. Antimicrobial and biodegradability were also screened.La reacción de cloruro de 2-hidroxiheptadecanoilo (2 con ácido antranílico produjo 2-(1-hidroxiheptadecil-4H-3,1-benzoxazin-4-ona (3 que fue usada como material de partida en la síntesis de compuestos heterocíclicos condensados y no condensados por reacción con nucleófilos nitrogenados (hidracina y formamida. La reacción de los productos sintetizados con distintas cantidades de óxido de propileno dio un grupo nuevo de compuestos no iónicos con una función doble como antibacterianos y agentes tensioactivos que pueden servir en la manufactura de medicamentos, cosméticos, pesticidas, o como productos antibacterianos y/o antifúngicos. Se determinaron las propiedades tensioactivas así como la capacidad antimicrobiana y la biodegrabilidad de los compuestos sintetizados.

  10. Molten salts activated by high-energy milling: A useful, low-temperature route for the synthesis of multiferroic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Hernández-Ramírez, Anayantzin; Martínez-Luévanos, Antonia [Facultad de Ciencias Químicas, Universidad Autónoma de Coahuila, V. Carranza s/n, Saltillo, Coahuila 25280 (Mexico); Fuentes, Antonio F. [CINVESTAV Unidad Saltillo, Apdo. Postal 663, Saltillo, Coahuila 25000 (Mexico); Earth and Environmental Science, University of Michigan, 3514 C.C. Little Building, 1100 N. University Avenue, Ann Arbor, MI 48109-1005 (United States); Nelson, Anna-Gay D.; Ewing, Rodney C. [Earth and Environmental Science, University of Michigan, 3514 C.C. Little Building, 1100 N. University Avenue, Ann Arbor, MI 48109-1005 (United States); Montemayor, Sagrario M., E-mail: smmontemayor@gmail.com [Facultad de Ciencias Químicas, Universidad Autónoma de Coahuila, V. Carranza s/n, Saltillo, Coahuila 25280 (Mexico); Earth and Environmental Science, University of Michigan, 3514 C.C. Little Building, 1100 N. University Avenue, Ann Arbor, MI 48109-1005 (United States)

    2014-01-25

    Highlights: • The synthesis route purposed demonstrates the formation of BiFeO{sub 3} at only 500 °C. • The magnetic and ferroelectric properties are comparable to those of bulk BiFeO{sub 3}. • By this route, several phases in Bi{sub 1−x}La{sub x}FeO{sub 3} system are obtained at only 500 °C. • The route developed here could be useful to synthesize other perovskite-type oxides. -- Abstract: There are only a few multiferroic compounds, among which BiFeO{sub 3} is the most important. Research the synthesis of bismuth ferrite, with novel and improved magnetic and electrical properties, has been mainly based on the use of hydrothermal or sol gel methods. However, these methods require either rather extreme conditions or several steps for synthesis. We demonstrate that the use of molten salts, activated by high energy milling, results in pure nanometric BiFeO{sub 3}, LaFeO{sub 3} and intermediate phases in the Bi{sub 1−x}La{sub x}FeO{sub 3} system. The chemical reagents used are Bi(NO{sub 3}){sub 3}⋅5H{sub 2}O, La(NO{sub 3}){sub 3}⋅6H{sub 2}O, Fe(NO{sub 3}){sub 3}⋅9H{sub 2}O and NaOH. A brief milling process of the reagents creates an amorphous precursor and crystalline NaNO{sub 3}. The thermal treatment of the precursors, at 500 °C for two hours, produces a crystalline mixture of Bi{sub 1−x}La{sub x}FeO{sub 3} and NaNO{sub 3}. Simple washing eliminates the NaNO{sub 3}. The characterization of intermediates and final products, through thermal analysis, X-ray diffraction and scanning electronic microscopy, allows the inference of possible mechanism. In addition, vibrating sample magnetometry (VSM) and ferroelectric tests show the typical magnetic and electric polarization loops characteristic of these materials even when formed at the nano-scale.

  11. Thiophene-containing Pechmann dyes and related compounds: synthesis, and experimental and DFT characterisation.

    Science.gov (United States)

    Kantchev, Eric Assen B; Norsten, Tyler B; Tan, Marilyn L Y; Ng, Joey J Y; Sullivan, Michael B

    2012-01-09

    Attaching 2-thienyl residues to the Pechmann dye core chromophore (5,5-exo-dilactone situated around a C-C double bond) results in a novel magenta-coloured compound (UV/Vis spectroscopy λ(max) =570 nm in CHCl(3)), which can be rearranged to a yellow 6,6-endo-dilactone (λ(max) =462 nm in CHCl(3)). Single and double amidation results in pronounced redshift in the 5,5-exo series (violet, λ(max) =570 nm and blue, λ(max) =606 nm in CHCl(3), respectively) but pronounced blueshift in the 6,6-endo series (yellow, λ(max) =424 nm and pale yellow bordering on colourless, λ(max) =395 nm in CHCl(3), respectively). Incorporation of a 3-alkyl substituent on the thiophene ring allows for sharp increase of solubility in organic solvents concomitant with fine-tuning of the colour: a redshift in 5,5-exo-dilactones but a blueshift in 5,5-exo-dilactams. DFT computations demonstrate that both lactone classes are planar regardless of the presence of a 3-alkyl group. The lactam derivatives are non-planar: the thiophene-core chromophore dihedral angles increase on going from 5,5-exo to 6,6-endo and from thiophene to 3-alkyl thiophene. Depending on the core heteroatom (O vs. N-alkyl), ring junction (5,5-exo vs. 6,6-endo) and 3-thiophene substituent (H vs. alkyl), two, three, four or six conformers are possible. All of these conformers were characterised by DFT and were found to be very close in energy at both IEFPCM/B3LYP/DGDZVP and SMD/M06/DGDZVP levels of theory. Within each conformer set, the HOMO and LUMO energies were within 0.05 eV and the predicted λ(max) values (TD-DFT) within 10 nm, and this implies low sensitivity of the optical and electronic properties to conformation. Cyclic voltammetry measurements of selected compounds demonstrated good matching to the HOMO and LUMO energies from IEFPCM/B3LYP/DGDZVP computations. M06-2X was the best DFT functional for TD-DFT, giving predicted λ(max) values within about 20 nm.

  12. Synthesis and Characterization of a New Triple-layered Perovskite KSr2Nb3O10 and Its Protonated Compounds

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    New layered perovskites, KSr2Nb3O10 and two new protonated niobates HSr2Nb3O10*1.2H2O and HSr2Nb3O10,were synthesized by solid state reaction and ion-exchange reaction.These new compounds were characterized by EPMA,AAS,XRD,IR,DTA and so on.The structure may be described as treble perovskite sheets [Sr2Nb3O10]- interleaved with K+,H3O+ or H+.These new compounds are new members of the Dion-Jacobsonseries with n=3 for the general formula M[An-1NbnO3n+1],and their indexed X-ray powder diffraction data were first reported in the paper.

  13. Synthesis of a new class of strongly fluorescent heterocyclic compounds: 3H-imidazo[4,5-a]acridine-11-carbonitriles

    Energy Technology Data Exchange (ETDEWEB)

    Sahraei, Robabeh [Department of Chemistry, Mashhad Branch, Islamic Azad University, Mashhad (Iran, Islamic Republic of); Pordel, Mehdi, E-mail: mehdipordel58@yahoo.com [Department of Chemistry, Mashhad Branch, Islamic Azad University, Mashhad (Iran, Islamic Republic of); Behmadi, Hossein; Razavi, Bahareh [Department of Chemistry, Mashhad Branch, Islamic Azad University, Mashhad (Iran, Islamic Republic of)

    2013-04-15

    The synthesis, spectral characterization and fluorescence studies of some novel substituted 8-chloro-3H-imidazo[4,5-a]acridine-11-carbonitriles are presented. The nucleophilic substitution of hydrogen in 5-nitrobenzimidazole derivatives occurs upon reaction with 2-(4-chlorophenyl) acetonitrile under basic conditions and proceeds with concomitant cyclisation. This sequence offers a one-pot synthesis of new fluorescent heterocyclic compounds, 8-chloro-3-alkyl-3H-imidazo[4,5-a]acridine-11-carbonitriles. The fluorescence of all compounds was intense and fluorescence quantum yields were very high (>0.85) for all of them. -- Highlights: ► A facile method to synthesis of new 3H-imidazo[4,5–a]acridine-11-carbonitriles is presented. ► The spectral and photophysical properties of these new compounds are investigated. ► The fluorescence of all compounds was intense and fluorescence quantum yields were very high for all of them.

  14. Synthesis and reactivity of single-phase Be{sub 17}Ti{sub 2} intermetallic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jae-Hwan, E-mail: kim.jaehwan@jaea.go.jp [Breeding Functional Materials Development Group, Sector of Fusion Research and Development, Japan Atomic Energy Agency (Japan); Iwakiri, Hirotomo; Furugen, Tatsuaki [Faculty of Education Elementary and Secondary School Teacher Training Program, University of the Ryukyus, Okinawa (Japan); Nakamichi, Masaru [Breeding Functional Materials Development Group, Sector of Fusion Research and Development, Japan Atomic Energy Agency (Japan)

    2016-01-15

    Highlights: • Preliminary synthesis of single-phase Be{sub 17}Ti{sub 2} was succeeded. • Reactivity difference between beryllium and beryllides may be caused by a lattice strain. • Oxidation of Be{sub 17}Ti{sub 2} at high temperatures results in the formation of TiO{sub 2}. • Simulation results reveal that a stable site for hydrogen at the center of tetrahedron exists. - Abstract: To investigate feasibility for application of Be{sub 17}Ti{sub 2} as a neutron multiplier as well as a refractory material, single-phase Be{sub 17}Ti{sub 2} intermetallic compounds were synthesized using an annealing heat treatment of the starting powder and a plasma sintering method. Scanning electron microscopic observations and X-ray diffraction measurements reveal that the single-phase Be{sub 17}Ti{sub 2} compounds were successfully synthesized. We examined the reactivity of Be{sub 17}Ti{sub 2} with 1% H{sub 2}O and discovered that a larger stoichiometric amount of Ti resulted in the formation of TiO{sub 2} on the surface at high temperatures. This oxidation may also contribute to an increase in both weight gain and generation of H{sub 2}. This suggests that the formation of the Ti-depleted Be{sub 17}Ti{sub 2−x} layer as a result of oxidation facilitates an increased reactivity with H{sub 2}O. To evaluate the safety aspects of Be{sub 17}Ti{sub 2}, we also investigated the hydrogen positions and solution energies based on the first principle. The calculations reveal that there are 10 theoretical sites, where 9 of these sites have hydrogen solution energies with a positive value (endothermic) and 1 site located at the center of a tetrahedron comprising two Be and two Ti atoms gives a negative value (exothermic).

  15. Palladium-catalyzed addition of potassium aryltrifluoroborates to aliphatic nitriles: synthesis of alkyl aryl ketones, diketone compounds, and 2-arylbenzo[b]furans.

    Science.gov (United States)

    Wang, Xingyong; Liu, Miaochang; Xu, Long; Wang, Qingzong; Chen, Jiuxi; Ding, Jinchang; Wu, Huayue

    2013-06-07

    A palladium-catalyzed addition of potassium aryltrifluoroborates to aliphatic nitriles has been developed, leading to a wide range of alkyl aryl ketones with moderate to excellent yields. Moreover, several dinitriles (e.g., malononitrile, glutaronitrile, and adiponitrile) were applicable to this process for the construction of 1,3-, 1,5-, or 1,6-dicarbonyl compounds. The scope of the developed approach is successfully explored toward the one-step synthesis of 2-arylbenzo[b]furans via sequential addition and intramolecular annulation reactions. The methodology accepted a wide range of substrates and is applicable to library synthesis.

  16. Synthesis and crystal structure of new K and Rb selenido/tellurido ferrate cluster compounds

    Energy Technology Data Exchange (ETDEWEB)

    Stueble, Pirmin; Berroth, Angela; Roehr, Caroline [Freiburg Univ. (Germany). Inst. fuer Anorganische und Analytische Chemie

    2016-08-01

    In the course of a systematic study of alkali iron chalcogenido salts containing clusters [Fe{sub 4}Q{sub 8}] a series of new mixed-valent potassium and rubidium selenido and tellurido ferrates(II/III) was synthesized by carefully heating the pure elements enclosed in sample tubes under an argon atmosphere up to maximum temperatures of 800-900 C. Their crystal structures have been determined by means of single crystal X-ray diffraction. The mixed-valent Fe{sup II/III} tellurido ferrates A{sub 7}[Fe{sub 4}Te{sub 8}] form three different structure types. All structures contain tetramers of four edge sharing [FeTe{sub 4}] tetrahedra, which are connected by common edges to form only slightly distorted tetrahedral [Fe{sub 4}Te{sub 8}]{sup 7-} anions ('stella quadrangula') with a [Fe{sub 4}Te{sub 4}] cubane core. In all cases, these anions are surrounded by 26 alkali cations, which are located at the eight corners and the midpoints of the six faces and 12 edges of a cube. The three crystal structures can thus be described by three different packings of cuboid moieties: The monoclinic rubidium compound Rb{sub 7}[Fe{sub 4}Te{sub 8}] (space group C2/c, a = 2000.16(7), b = 897.79(3), c = 1768.12(6) pm, β = 117.4995(10) , Z = 4, R1 = 0.0296) is isotypic to the known cesium tellurido and sulfido ferrates Cs{sub 7}[Fe{sub 4}(S/Te){sub 8}]. Depending on the temperature, K{sub 7}[Fe{sub 4}Te{sub 8}] forms two different but closely related new structure types: The tetragonal r.t. modification (space group P4{sub 2}/nmc, a = 1222.25(14), c = 872.1(2) pm, Z = 2, R1 = 0.0583) crystallizes in a supergroup of the orthorhombic l.t. (100 K) form (space group Pbcn, a = 1715.5, b = 866.76(3), c = 1715.50(7) pm, Z = 4, R1 = 0.0160). In all structures, the cluster centered cubes are stacked to form columns along the short (∼ 870 pm) axis. These columns are themselves densely packed with 4 (both K compounds) and 6 (A = Rb) adjacent face-sharing columns. According to these

  17. Synthesis and crystal structure of the coordination compound of pyridoxine with manganese sulfate

    Science.gov (United States)

    Furmanova, N. G.; Verin, I. A.; Shyityeva, N.; Sulaimankulov, K. S.; Berdalieva, Zh.; Resnyanskii, V. F.; Duishenbaeva, A. T.

    2011-11-01

    The reaction of pyridoxine with manganese sulfate in an aqueous solution gave the coordination compound MnSO4 · 2C8H11O3N · 2H2O ( I). The structure of I was determined from single-crystal X-ray diffraction data. In the centrosymmetric complex (sp. gr. Pbar 1, Z = 1), the Mn atom is coordinated by two pyridoxine molecules and two water molecules, thus adopting an octahedral coordination. The sulfate anion is also at a center of symmetry and, consequently, is disordered. The pyridoxine molecules are coordinated to the metal atom through the oxygen atoms of the deprotonated hydroxyl group and the CH2OH group that retains the hydrogen atom. The nitrogen atom is protonated in such a way that the heterocycle assumes a pyridinium character. The crystal structure also contains six water molecules of crystallization. A thermogravimetric study showed that the decomposition of I occurs in several successive steps, such as dehydration, the combustion of organic ligands, and the formation of an inorganic residue.

  18. Synthesis and characterization of a strong-fluorescent Eu-containing hydrotalcite-like compound

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    A novel strong-fluorescent Eu-containing hydrotalcite-like compound (Eu-HTlc) was synthesized using the coprecipitation method,in which aluminum(III) was partially substituted by Europium (III) in the hydrotalcite-like layers,and thenoyltrifluoroacetone,1,10-phenanthroline were dispersed into the anions in the interlayer region.The sample was characterized by XRD,XPS,FT-IR,ICP,TG-DSC,TEM and fluorescence spectra,and its composition and structure were determined.The results indicated that the sample exhibited a characteristic red light (614 nm).The fluorescent lifetime and fluorescence quantum yield of Eu-HTlc were measured to be respectively 893 -s and 66.44%,higher than those of Eu(III)-thenoyltrifluoroacetone1,10-phenanthroline complex [Eu(TTA)3phen].The result of TG-DSC measurement showed the enhanced thermal stability of Eu-HTlc compared with that of MgAl-LDHs and Eu(TTA)3phen.With excellent photoluminescent property and thermal stability,low contents of rare earth ions and ligands,the Eu-HTlc may become one of the novel fluorescent materials with potential applications.

  19. Synthesis and structures of two cobalt compounds of 2-amino-2-methyl-1-propanol

    Indian Academy of Sciences (India)

    YONGJIE QIN; SHANSHAN YANG; LONG LIU; YUNING LIANG; ZILU CHEN

    2017-01-01

    The reactions of 2-amino-2-methyl-1-propanol (MepH) with Co(ClO₄) ₂•6H₂O in the presence of acetic acid gave [Co₂ (Mep) ₃ (OAc)(MepH)](ClO₄) ₂•MepH (1) and [CoIII ₄ CoII ₂ (Mep)8(μ₃-OH) ₂ (OAc) ₄](ClO₄) ₂• 2EtOH•2H₂O (2). They were characterized by elemental analysis, IR and single crystal X-ray diffraction analysis. Compound 1 presents a dinuclear structure with its two Co atoms linked by two Mep⁻ ligands and one acetate ligand. The two Co(II) and four Co(III) centers in 2 are held together by eight Mep⁻ ligands, two μ₃-OH⁻ ions and four acetate ligands to form a hexanuclear skeleton which contains a defected face-shared dicubane core. Their discrete polynuclear units are further linked into double-layered and mono-layered two-dimensional H-bonded framework, respectively.

  20. Synthesis, characterization, thermal and computational studies of novel tetra-azido compounds as energetic plasticizers

    Science.gov (United States)

    Baghersad, Mohammad Hadi; Habibi, Azizollah; Heydari, Akbar

    2017-02-01

    In this paper, four azido compounds have been synthesized and characterized as new energetic plasticizers. Nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy, elemental analysis, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and differential thermal analysis (DTA) have been used to identify and determine the properties of the synthesized plasticizers. The plasticization effect of plasticizers on glycidyl azide polymer (GAP) has been investigated by viscosity measurements and thermal analysis of the prepolymer-plasticizer mixtures and plasticized binders. The plasticized mixtures were cured by a diisocyanate curing agent and the glass transition temperature and decomposition temperature of the cured polyurethane binders were measured. Thermal analysis of the prepolymer-plasticizer and cured polymer mixtures showed that the synthesized plasticizers are completely compatible with the GAP binder and have a very good plasticizing effect. Furthermore, equilibrium geometry and heats of formation of each of the plasticizer molecules were obtained using the thermochemical T1 recipe, which is available in wave function Spartan software. Comparing empirical heats of combustion and calculated heats of combustion by using the heats of formation showed that the suggested optimum molecular structure by the T1 recipe has a high similarity to the real molecular structure of these molecules.

  1. Synthesis and Crystal Structure of Copper(Ⅱ) Compound with Didentate Schiff-base Ligand

    Institute of Scientific and Technical Information of China (English)

    易龙; 丁斌; 程鹏

    2004-01-01

    The title complex [Cu(L)2] (HL=4-salicylideneamino-3,5-dimethanol-1,2,4-triazole) was synthesized by the reaction of Cu(CH3COO)2·2H2O with 4-salicylideneamino-3,5-dimethanol- 1,2,4-triazole in the methanol. The single-crystal X-ray study reveals that the compound crystallizes in monoclinic, space group P21/n with a = 11.746(5), b = 8.145(3), c = 12.786(5)A,β = 106.64(1)°, V = 1172(1)A3, Z = 2, Dc = 1.581 g/cm3, μ= 0.989 mm-1, F(000) = 574, C22H22Cu- N8O6, Mr = 558.02, T = 293(2) K, R = 0.0394 and Rw = 0.0835 for 2376 observed reflections with I > 2σ(I). The complex comprises a four-coordinated copper(Ⅱ) center, with an N2O2 planar coordi- nation environment. The molecules are connected by hydrogen bonds to form one-dimensional chains which are further linked to form a two-dimensional plane.

  2. Microwave: An Important and Efficient Tool for the Synthesis of Biological potent Organic Compounds.

    Science.gov (United States)

    Kumari, Kamlesh; Vishvakarma, Vijay K; Singh, Prashant; Patel, Rajan; Chandra, Ramesh

    2017-05-28

    Green Chemistry is an interdisciplinary science or can also be explained as a branch of chemistry. It is generally described as the chemistry to aim to synthesize chemical compounds to trim down the utilization of harmful chemicals proposed by the Environmental Protection Agency (EPA). Recently, the plan of academicians, researchers, industrialists is to generate greener and more efficient methodologies to carry out various organic syntheses. In the present scenario, green chemistry utilizes the raw materials economically, minimizes the waste and prevents the uses of harmful or hazardous chemicals to make the organic reactions simple and efficient. Microwave technique is a new simple and efficient technology which opens new prospects to the chemist to carry out various reactions, which are difficult using conventional methodology. It is used to decrease the duration of time to carry various organic transformation along with maximum yield, minimum by-products, minimum energy utilization, less manpower etc. e.g. various famous organic reactions have been carried out by various research groups like Aldol condensation, Knoevenagel condensation, Beckmann rearrangement, Vilsmeier reaction, Perkin reaction, Benzil-Benzilic acid rearrangement, Fischer cyclization, Mannich reaction, Claisen-Schmidt condensation, etc. Further, reduction, oxidation, coupling, condensation reaction were also performed using microwave technology. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  3. Synthesis and Thermal Decomposition Mechanism of the Energetic Compound 3,5-Dinitro-4-nitroxypyrazole

    Science.gov (United States)

    Feng, Xiao-Qin; Cao, Duan-Lin; Cui, Jian-Lan

    2016-07-01

    A novel energetic material, 3,5-dinitro-4-nitroxypyrazole (DNNP), was synthesized via nitration and nucleophilic substitution reaction using 4-chloropyrazole as raw material. The structure of DNNP was characterized by Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR), and elemental analysis. Its detonation properties were calculated and compared with those of other commonly used energetic compounds. The thermal decomposition mechanism of DNNP was studied by means of thermogravimetry and differential scanning calorimetry coupled with a mass spectrometry (DSC-MS). The results show that the detonation properties of DNNP were better than those of TNT and comparable to those of 1,3,5-trinitroperhydro-1,3,5-triazine (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX). In addition, the thermal decomposition mechanism of DNNP was supposed. Initially, the O-NO2 bond was broken, thereby producing a nitropyrazole oxygen radical. Subsequently, the nitropyrazole oxygen radical was decomposed by free radical cleavage of nitro or isomerized to nitritepyrazole and subsequently decomposed by free radical cleavage of the nitroso group. Finally, pyrazole ring fission occurred and produced N2, NO, N2O, and CO2.

  4. Radiolysis compounds in bacon and chicken. Final report 18 Sep 81-20 Sep 82

    Energy Technology Data Exchange (ETDEWEB)

    Merritt, C. Jr.

    1984-01-01

    The results of this study are in agreement with the precepts established in studies published previously on beef, chicken, ham, and pork. The radiolysis compounds from bacon, chicken, ham, and pork are comparable in identity and amounts to those found in irradiated beef for comparable compositions and irradiation parameters (temperature, dose, etc.). The results of this study support the conclusions drawn in the CORC report of 'commonality in chemistry, predictability of products, and extrapolation of results.' Consequently, the same conclusions can be drawn concerning the wholesomeness of irradiated bacon, chicken, ham, and pork as for other irradiated meat products of similar composition and irradiation parameters as reported in the FASEB report and its supplements (I and II) on irradiated beef.

  5. A facile synthesis of new 5-aryl-thiophenes bearing sulfonamide moiety via Pd(0-catalyzed Suzuki–Miyaura cross coupling reactions and 5-bromothiophene-2-acetamide: As potent urease inhibitor, antibacterial agent and hemolytically active compounds

    Directory of Open Access Journals (Sweden)

    Mnaza Noreen

    2017-01-01

    Full Text Available The present study reports a convenient approach for the synthesis of thiophene sulfonamide derivatives (3a–3k via Suzuki cross coupling reaction. This method of synthesis involved the reactions of various aryl boronic acids and esters with 5-bromthiophene-2-sulfonamide (2 under mild and suitable temperature conditions. The compounds synthesized in the present study were subjected to urease inhibition and hemolytic activities. The substitution pattern and the electronic effects of different functional groups (i.e., Cl, CH3, OCH3, F etc. available on the aromatic ring are found to have significant effect on the overall results. The compound 5-Phenylthiophene-2-sulfonamide 3a showed the highest urease inhibition activity with IC50 value ∼ 30.8 μg/mL compared with the thiourea (used as standard having IC50 value ∼ 43 μg/mL. Moreover, almost all of the compounds were examined for the hemolytic activity against triton X-100 with positive results obtained in most of the cases. In addition, the antibacterial activities of the derivatives of 5-arylthiophene-2-sulfonamide and 5-bromothiophene-2-acetamide were also investigated during the course of the study.

  6. Synthesis of CdTe QDs/single-walled aluminosilicate nanotubes hybrid compound and their antimicrobial activity on bacteria

    Energy Technology Data Exchange (ETDEWEB)

    Geraldo, Daniela A., E-mail: daniela.geraldo@unab.cl [Universidad Andres Bello, Departamento de Ciencias Quimicas (Chile); Arancibia-Miranda, Nicolas [CEDENNA, Center for the Development of Nanoscience and Nanotechnology (Chile); Villagra, Nicolas A. [Universidad Andres Bello, Laboratorio de Microbiologia, Facultad de Ciencias Biologicas (Chile); Mora, Guido C. [Universidad Andres Bello, Unidad de Microbiologia, Facultad de Medicina (Chile); Arratia-Perez, Ramiro [Universidad Andres Bello, Departamento de Ciencias Quimicas (Chile)

    2012-12-15

    The use of molecular conjugates of quantum dots (nanocrystalline fluorophores) for biological purposes have received much attention due to their improved biological activity. However, relatively, little is known about the synthesis and application of aluminosilicate nanotubes decorated with quantum dots (QDs) for imaging and treatment of pathogenic bacteria. This paper describes for a first time, the use of single-walled aluminosilicate nanotubes (SWNT) (imogolite) as a one-dimensional template for the in situ growth of mercaptopropionic acid-capped CdTe QDs. This new nanohybrid hydrogel was synthesized by a simple reaction pathway and their enhanced optical properties were monitored by fluorescence and UV-Vis spectroscopy, confirming that the use of these nanotubes favors the confinement effects of net CdTe QDs. In addition, studies of FT-IR spectroscopy and transmission electron microscopy confirmed the non-covalent functionalization of SWNT. Finally, the antimicrobial activity of SWNT coated with CdTe QDs toward three opportunistic multi-resistant pathogens such as Salmonella typhimurium, Acinetobacter baumannii, and Pseudomonas aeruginosa were tested. Growth inhibition tests were conducted by exposing growing bacteria to CdTe QDs/SWNT hybrid compound showing that the new nano-structured composite is a potential antimicrobial agent for heavy metal-resistant bacteria.

  7. Photoaddition reactions of silyl ketene acetals with aromatic carbonyl compounds: a new procedure for {beta}-hydroxyester synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Ung Chan; Kim, Moon Jung; Moon, Jae Joon; Oh, Sun Wha; Kim, Hyun Jin [Pusan National Univ., Pusan (Korea, Republic of); Mariano, Patrick S. [University of New Mexico, Albuquerque (United States)

    2002-09-01

    Photochemical reactions of aromatic carbonyl compounds with silyl ketene acetals have been explored. Irradiation of acetonitrile or benzene solutions containing aryl aldehydes or ketones in the presence of silyl ketene acetals is observed to promote formation of {beta}-hydroxyester, 2,2-dioxyoxetane and 3,3-dioxyoxetane products. The ratios of these photoproducts, which arise by competitive single electron transfer (SET) and classical Paterno-Buchi mechanistic pathway, is found to be dependent on the degree of methyl-substitution on the vinyl moieties of the ketene acetals in a manner which reflects expected alkyl substituent effects on the oxidation potentials of these electron rich donors. An analysis of the product distribution arising by irradiation of a solution containing butyrophenone (6) and the silyl ketene acetal 9, derived from methyl isobutyrate, provides an estimate of the rate constants for the competitive Norrish type II, SET and Paterno-Buchi processes occurring. Finally, sequences involving silyl ketene acetal-aryl aldehyde or ketone photoaddition followed by 2,2-dioxyoxetane hydrolysis represent useful procedures for Claisen-condensation type, {beta}-hydroxyester synthesis.

  8. Synthesis and structural, magnetic, and resonance properties of the LiCuFe2(VO4)3 compound

    Science.gov (United States)

    Drokina, T. V.; Petrakovskii, G. A.; Bayukov, O. A.; Vorotynov, A. M.; Velikanov, D. A.; Molokeev, M. S.

    2016-10-01

    Complex studies have been performed for the structural, static magnetic, and resonance properties of a new magnet LiCuFe2(VO4)3 prepared by solid-phase synthesis. The temperature dependence of the susceptibility has an anomaly at temperature T max = 9.6 K. At high temperatures, the LiCuFe2(VO4)3 sample is in the paramagnetic state described by the Curie-Weiss law at T > 50 K and mainly determined by iron ions with effective magnetic moment μeff(exp) = 8.6μB per formula unit. At low temperatures, a long-range magnetic order is observed in the magnetic subsystem of the sample; the order is predominantly characterized by the antiferromagnetic exchange interaction and high frustration level. The exchange interaction parameters are estimated in a six-sublattice representation of the LiCuFe2(VO4)3 magnet. It is shown that the LiCuFe2(VO4)3 compound is an antiferromagnet with strong intrachain and frustrating interchain exchange interactions.

  9. Solvent Extraction of Chemical Attribution Signature Compounds from Painted Wall Board: Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Wahl, Jon H.; Colburn, Heather A.

    2009-10-29

    This report summarizes work that developed a robust solvent extraction procedure for recovery of chemical attribution signature (CAS) compound dimethyl methyl phosphonate (DMMP) (as well as diethyl methyl phosphonate (DEMP), diethyl methyl phosphonothioate (DEMPT), and diisopropyl methyl phosphonate (DIMP)) from painted wall board (PWB), which was selected previously as the exposed media by the chemical attribution scientific working group (CASWG). An accelerated solvent extraction approach was examined to determine the most effective method of extraction from PWB. Three different solvent systems were examined, which varied in solvent strength and polarity (i.e., 1:1 dichloromethane : acetone,100% methanol, and 1% isopropanol in pentane) with a 1:1 methylene chloride : acetone mixture having the most robust and consistent extraction for four original target organophosphorus compounds. The optimum extraction solvent was determined based on the extraction efficiency of the target analytes from spiked painted wallboard as determined by gas chromatography x gas chromatography mass spectrometry (GCxGC-MS) analysis of the extract. An average extraction efficiency of approximately 60% was obtained for these four compounds. The extraction approach was further demonstrated by extracting and detecting the chemical impurities present in neat DMMP that was vapor-deposited onto painted wallboard tickets.

  10. Synthesis and analgesic profile of conformationally constrained N-acylhydrazone analogues: discovery of novel N-arylideneamino quinazolin-4(3H)-one compounds derived from natural safrole.

    Science.gov (United States)

    Maia, Rodolfo C; Silva, Leandro L; Mazzeu, Eduardo F; Fumian, Milla M; de Rezende, Claudia M; Doriguetto, Antonio C; Corrêa, Rodrigo S; Miranda, Ana Luisa P; Barreiro, Eliezer J; Fraga, Carlos Alberto Manssour

    2009-09-15

    In this work we reported the synthesis and evaluation of the analgesic, anti-inflammatory, and platelet anti-aggregating properties of new 3-(arylideneamino)-2-methyl-6,7-methylenedioxy-quinazolin-4(3H)-one derivatives (3a-j), designed as conformationally constrained analogues of analgesic 1,3-benzodioxolyl-N-acylhydrazones (1) previously developed at LASSBio. Target compounds were synthesized in very good yields exploiting abundant Brazilian natural product safrole (2) as starting material. The pharmacological assays lead us to identify compounds LASSBio-1240 (3b) and LASSBio-1272 (3d) as new analgesic prototypes, presenting an antinociceptive profile more potent and effective than dipyrone and indomethacin used, respectively, as standards in AcOH-induced abdominal constrictions assay and in the formalin test. These results confirmed the success in the exploitation of conformation restriction strategy for identification of novel cyclic N-acylhydrazone analogues with optimized analgesic profile.

  11. Synthesis and optical properties of biphenylene ethynylene co-polymers and their model compounds

    Indian Academy of Sciences (India)

    Okhil K Nag; Kazi M Anis-Ul-Haque; Dipen Debnath; Rockshana Begum; Muhammad Younus; Nazia Chawdhury; Gabriele Kociok-Köhn; Paul R Raithby

    2015-03-01

    A new series of biphenylene ethynylene co-polymers, poly(2,5-dialkoxy-4-phenyleneethynylene-4,4-biphenyleneethynylene)s of the general formula [-C≡-4-C6H4-C6H4-4-C≡C-C6H2(2,5-OR)2-]n (R=C4H9 P1, C8H17 P2) has been synthesized using a palladium/copper catalyzed coupling reaction between HC≡-4-C6H4-C6H4-4-C≡C-H and IC6H2(2,5-OR)2I. The new co-polymer [-C≡C-C6H2(2,5-OC8H17)2-C≡C-C6H2(2,5-OC4H9)2-]n P5 has also been formed where different alkoxy substituents are present on alternate arene rings in the same polymer backbone. All the polymers were characterized by IR, 1H and 13C NMR spectroscopy and by GPC. The model compounds C6H5-4-C6H4-C≡C-C6H2(2,5-OR)2-4-C6H4-C6H5 (R=C4H9 M1, C8H17 M2) have also been prepared by the reaction between C6H5-4-C6H4-C≡CH and IC6H2(2,5-OR)2I. Single crystal X-ray structures of M1, M2 and Me3Si-C≡C-4-C6H4-C6H4-4-C≡CSiMe3 were determined with a view to obtain a better understanding of the molecular and intermolecular interactions in the solid state which has been used to explain the optical properties of the polymers derived from them. The absorption and photoluminescence spectra of the polymers, P1, P2 and P5 showed that the lowest energy band is blue shifted due to the introduction of biphenylene fragments into the alkoxy substituted poly(ethynylenephenylene)s.

  12. Computer-aided identification, design and synthesis of a novel series of compounds with selective antiviral activity against chikungunya virus.

    Science.gov (United States)

    Bassetto, Marcella; De Burghgraeve, Tine; Delang, Leen; Massarotti, Alberto; Coluccia, Antonio; Zonta, Nicola; Gatti, Valerio; Colombano, Giampiero; Sorba, Giovanni; Silvestri, Romano; Tron, Gian Cesare; Neyts, Johan; Leyssen, Pieter; Brancale, Andrea

    2013-04-01

    Chikungunya virus (CHIKV) is an Arbovirus that is transmitted to humans primarily by the mosquito species Aedes aegypti. Infection with this pathogen is often associated with fever, rash and arthralgia. Neither a vaccine nor an antiviral drug is available for the prevention or treatment of this disease. Albeit considered a tropical pathogen, adaptation of the virus to the mosquito species Aedes albopictus, which is also very common in temperate zones, has resulted in recent outbreaks in Europe and the US. In the present study, we report on the discovery of a novel series of compounds that inhibit CHIKV replication in the low μM range. In particular, we initially performed a virtual screening simulation of ∼5 million compounds on the CHIKV nsP2, the viral protease, after which we investigated and explored the Structure-Activity Relationships of the hit identified in silico. Overall, a series of 26 compounds, including the original hit, was evaluated in a virus-cell-based CPE reduction assay. The study of such selective inhibitors will contribute to a better understanding of the CHIKV replication cycle and may represents a first step towards the development of a clinical candidate drug for the treatment of this disease.

  13. Synthesis, molecular structure and magnetic properties of a rhenium(IV) compound with catechol

    Science.gov (United States)

    Cuevas, A.; Geis, L.; Pintos, V.; Chiozzone, R.; Sanchíz, J.; Hummert, M.; Schumann, H.; Kremer, C.

    2009-03-01

    A novel Re(IV) complex containing catechol as ligand has been prepared and characterized. The crystal structure of (HNEt 3)(NBu 4)[ReCl 4(cat)]·H 2cat was determined. The rhenium ion presents a distorted octahedral geometry, being bonded to a bidentate catecholate group and four chloride anions. The magnetic properties of the complex were studied, a /2 D/ (the energy gap between ±3/2 and ±1/2 Kramers doublets) value of 190(10) cm -1. This is the largest /2 D/ value reported for Re(IV) up to now.

  14. Palladium-catalysed cyclisation of alkenols: Synthesis of oxaheterocycles as core intermediates of natural compounds

    Directory of Open Access Journals (Sweden)

    Miroslav Palík

    2014-09-01

    Full Text Available The study of Pd-catalysed cyclisation reactions of alkenols using different catalytic systems is reported. These transformations affect the stereoselective construction of mono- and/or bicyclic oxaheterocyclic derivatives depending on a starting alkenol. The substrate scope and proposed mechanism of Pd-catalysed cyclisation reactions are also discussed. Moreover, the diastereoselective Pd-catalysed cyclisation of appropriate alkenols to tetrahydrofurans and subsequent cyclisation provided properly substituted 2,5-dioxabicyclo[2.2.1]heptane and 2,6-dioxabicyclo[3.2.1]octane, respectively. Such bicyclic ring subunits are found in many natural products including ocellenynes and aurovertines.

  15. Synthesis and Electronic Structure of Ru2(Xap)4(Y-gem-DEE) Type Compounds: Effect of Cross-Conjugation.

    Science.gov (United States)

    Forrest, William P; Choudhuri, Mohommad M R; Kilyanek, Stefan M; Natoli, Sean N; Prentice, Boone M; Fanwick, Phillip E; Crutchley, Robert J; Ren, Tong

    2015-08-03

    Reported in this Article are the preparation and characterization of a series of new Ru2(II,III) compounds bearing one cross-conjugated σ-geminal-diethynylethene ligand (gem-DEE), namely, Ru2(Xap)4(Y-gem-DEE) (Xap = N,N'-anilinopyridinate (ap) or 2-(3,5-dimethoxy)anilinopyridinate (DiMeOap), and Y = Si(i)Pr3 (1) or H (2)) and [Ru2(ap)4]2(μ-gem-DEE) (3). Compounds 1-3 were characterized by spectroscopic and voltammetric techniques as well as the single crystal X-ray diffraction study of 2a. The X-ray structural data of 2a and the spectroscopic/voltammetric data of compounds 1 and 2 indicate that the gem-DEE ligands are similar to simple alkynyls in their effects on the molecular and electronic structures of the Ru2(Xap)4 moiety. Similar to the previously studied [Ru2(ap)4]2(μ-C2n) type compounds, dimer 3 exhibits pairwise 1e(-) oxidations and reductions, albeit the potential splits within the pair (ΔE1/2) are significantly smaller than those of [Ru2(ap)4]2(μ-C4). The electronic absorption spectra of the reduced and oxidized derivatives of 1a and 3 were determined using spectroelectrochemistry methods. No discernible intervalence charge transfer transition (IVCT) was detected in the near-IR spectrum for either 3(-) or 3(+), suggesting that the Ru2-Ru2 coupling in these mixed-valence states is weak. DFT calculations on a model compound of 3 yielded six singly occupied molecular orbitals (SOMOs), which have Ru2 contributions similar to those previously calculated for the [Ru2(ap)4]2(μ-C2n) type compounds. Among six SOMOs, SOMO-2 is the only one containing substantial dπ-π(gem-DEE) character across the entire Ru2-μ-gem-DEE-Ru2 linkage, which explains the weakened Ru2-Ru2 coupling.

  16. A novel process for methanol synthesis. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Tierney, J.W.; Wender, I.

    1994-01-25

    The use of methanol (MeOH) as a fuel additive and in MTBE production has renewed interest in the search for improved MeOH processes. Commercial processes are characterized by high pressures and temperatures with low per pass conversion (10--12%). Efforts are underway to find improved MeOH synthesis processes. A slurry phase ``concurrent`` synthesis of MeOH/methyl formate (MeF) which operates under relatively mild conditions (100{degrees}C lower than present commercial processes) was the subject of investigation in this work. Evidence for a reaction scheme involving the carbonylation of MeOH to MeF followed by the hydrogenolysis of MeF to two molecules of MeOH -- the net result being the reaction of H{sub 2} with CO to give MeOH via MeF, is presented. Up to 90% per pass conversion and 98% selectivity to methanol at rates comparable to commercial processes have been obtained in spite of the presence of as much as 10,000 ppM CO{sub 2} and 3000 ppM H{sub 2}O in the gas and liquid respectively. The effect of process parameters such as temperature, pressure, H{sub 2}/CO ratio in the reactor, flow rate and catalyst loading were also investigated. The use of temperatures above 170{degrees}C at a pressure of 50 atm results in MeF being the limiting reactant. Small amounts of CH{sub 4} are also formed. Significant MeOH synthesis rates at a pressure in the range of 40--50 atm makes possible the elimination of an upstream shift reactor and the use of an air-blown syngas generator. The nature of the catalysts was studied and correlated with the behavior of the various species in the concurrent synthesis.

  17. Enantioselective Synthesis of α-Mercapto-β-amino Esters via Rh(II)/Chiral Phosphoric Acid-Cocatalyzed Three-Component Reaction of Diazo Compounds, Thiols, and Imines.

    Science.gov (United States)

    Xiao, Guolan; Ma, Chaoqun; Xing, Dong; Hu, Wenhao

    2016-12-02

    An enantioselective method for the synthesis of α-mercapto-β-amino esters has been developed via a rhodium(II)/chiral phosphoric acid-cocatalyzed three-component reaction of diazo compounds, thiols, and imines. This transformation is proposed to proceed through enantioselective trapping of the sulfonium ylide intermediate generated in situ from the diazo compound and thiol by the phosphoric acid-activated imine. With this method, a series of α-mercapto-β-amino esters were obtained in good yields with moderate to good stereoselectivities.

  18. Synthesis, crystal growth and characterization of a chiral compound (triphenylphosphine oxide cadmium iodide): A new semiorganic nonlinear optical material

    Science.gov (United States)

    Santhakumari, R.; Ramamurthi, K.; Stoeckli-Evans, Helen; Hema, R.; Nirmala, W.

    2011-05-01

    Synthesis of semiorganic material, triphenylphosphine oxide cadmium iodide (TPPOCdI), is reported for the first time. Employing the temperature reduction method, a crystal of size 16×7×6 mm 3 was grown from dimethyl sulfoxide (DMSO) solution. Three dimensional crystal structure of the grown crystal was determined by single crystal X-ray diffraction study. The complex crystallizes in the chiral orthorhombic space group P2 12 12 1. FTIR study was carried out in order to confirm the presence of the functional groups. UV-vis-NIR spectral studies show that the crystal is transparent in the wavelength range of 290-1100 nm. The microhardness test was carried out, and the load hardness was measured. Thermogravimetric and differential thermal analyses reveal the thermal stability of the crystal. Second harmonic generation efficiency of the powdered TPPOCdI, tested using Nd: YAG laser, is ∼0.65 times that of potassium dihydrogen orthophosphate.

  19. Reviews of the Norwegian climate policy - a synthesis of four international reports

    Energy Technology Data Exchange (ETDEWEB)

    Alfsen, Knut H.; Bjoernaes, Christian; Reed, Eilif Ursin

    2011-07-01

    The report is a synthesis of four reviews on the Norwegian climate policy: 1. Environmental performance review of Norway, OECD 2011 2. Energy Policies of IEA Countries, Norway, IEA 2011 3. Economic Survey of Norway, OECD 2010 4. Report on the in-depth review of the fifth national communication of Norway.(auth)

  20. Ecosystems and human well-being - Synthesis: A Report of the Millennium Ecosystem Assessment

    NARCIS (Netherlands)

    Reid, W.V.; Mooney, H.A.; Cropper, A.; Capistrano, D.; Carpenter, S.R.; Chopra, K.; Dasgupta, P.; Dietz, T.; Duraiappah, A.K.; Hassan, R.; Kasperson, R.; Leemans, R.; May, R.M.; McMichael, A.J.; Pingali, P.; Samper, C.; Scholes, R.; Watson, R.T.; Zakri, A.H.; Shidong, Z.; Ash, N.J.; Bennett, E.; Kumar, P.; Lee, M.J.; Raudsepp-Hearne, C.; Simons, H.; Thonell, J.; Zurek, M.B.

    2005-01-01

    This report presents a synthesis and integration of the findings of the four MA Working Groups (Condition and Trends, Scenarios, Responses, and Sub-global Assessments). It does not, however, provide a comprehensive summary of each Working Group report, and readers are encouraged to also review the f

  1. Detection of estrogenic activity in sediment-associated compounds using in vitro reporter gene assays.

    Science.gov (United States)

    Legler, Juliette; Dennekamp, Martine; Vethaak, A Dick; Brouwer, Abraham; Koeman, Jan H; van der Burg, Bart; Murk, Albertinka J

    2002-07-03

    Sediments may be the ultimate sink for persistent (xeno-)estrogenic compounds released into the aquatic environment. Sediment-associated estrogenic potency was measured with an estrogen receptor-mediated luciferase reporter gene (ER-CALUX) assay and compared with a recombinant yeast screen. The ER-CALUX assay was more sensitive to 17beta-estradiol (E2) than the recombinant yeast screen, with an EC50 of 6 pM E2 compared to 100 pM in the yeast screen. Yeast cells were unable to distinguish the anti-estrogens ICI 182,780 and (4-hydroxy)tamoxifen, which were agonistic in the yeast. Acetone-soluble fractions of hexane/acetone extracts of sediments showed higher estrogenic potency than hexane-soluble extracts in the ER-CALUX assay. Sediments obtained from industrialized areas such as the Port of Rotterdam showed the highest estrogenic potency of the 12 marine sediments tested (up to 40 pmol estradiol equivalents per gram sediment). The estrogenic activity of individual chemicals that can be found in sediments including: alkylphenol ethoxylates and carboxylates; phthalates; and pesticides, was tested. Increasing sidechain length of various nonylphenol ethoxylates resulted in decreased estrogenic activity. Of the phthalates tested, butylbenzylphthalate was the most estrogenic, though with a potency approximately 100,000 times less than E2. The organochlorine herbicides atrazine and simazine failed to induce reporter gene activity. As metabolic activation may be required to induce estrogenic activity, a metabolic transformation step was added to the ER-CALUX assay using incubation of compounds with liver microsomes obtained from PCB-treated rats. Results indicate that metabolites of E2, NP and bisphenol A were less active than the parent compounds, while metabolites of methoxychlor were more estrogenic following microsomal incubations.

  2. The catalysis of nucleotide polymerization by compounds of divalent lead. [prebiotic synthesis

    Science.gov (United States)

    Sleeper, H. L.; Orgel, L. E.

    1979-01-01

    The nonenzymatic, nontemplate catalysis of nucleotide polymerization by Pb(2+) ions, a possible prebiotic catalyst, is reported. Adenosine and uridine phosphoimidazoles were reacted in buffered solutions of lead salts and products were analyzed by means of paper chromatography and electrophoresis. In the presence of Pb(2+) ion at pH 8.0 and 7.0 the reaction is found to progress rapidly with excellent yields of oligomers, with optimal yields observed at pH 8.0. Little temperature dependence in the range 0 to 30 C is observed, however hydrolysis of the reaction products is minimal when the reaction is carried out at 0 C. Results show that the yield of oligomers is insensitive to mixing or the source of lead ions, indicating that naturally occurring minerals or precipitates could be a source of Pb(2+) ions under prebiotic conditions.

  3. Synthesis of Dichlorophosphinenickel(II) Compounds and Their Catalytic Activity in Suzuki Cross-Coupling Reactions: A Simple Air-Free Experiment for Inorganic Chemistry Laboratory

    Science.gov (United States)

    Thananatthanachon, Todsapon; Lecklider, Michelle R.

    2017-01-01

    In this experiment, students perform an air-free synthesis of three dichlorophosphinenickel(II) compounds, NiCl[subscript 2](PPh[subscript 3])[subscript 2], NiCl[subscript 2](PCy[subscript 3])[subscript 2], and NiCl[subscript 2](DPPE), using NiCl[subscript 2]·6H[subscript 2]O and the appropriate phosphine as the precursors. These colorful nickel…

  4. Hexamethylenetetramine reaction with graphite oxide (GO as a strategy to increase the thermal stability of GO: synthesis and characterization of a compound

    Directory of Open Access Journals (Sweden)

    ROBSON F. de FARIAS

    2010-04-01

    Full Text Available In this paper, the synthesis and characterization of a GO–hmta compound (GO – graphite oxide; hmta – hexamethylenetetramine are presented. It is shown that the presence of hmta molecules inside the GO matrix, with very strong interactions, stabilize the GO matrix from a thermal point of view. Such a fact could be used to explore possible applications of GO matrix, especially in catalysis.

  5. Hydrogen Release Compound (HRC®) Barrier Application At The North Of Basin F Site, Rocky Mountain Arsenal; Innovative Technology Evaluation Report

    Science.gov (United States)

    This Innovative Technology Evaluation Report documents the results of a demonstration of the hydrogen release compound (HRC®) barrier technology developed by Regenesis Bioremediation Products, Inc., of San Clemente, California. HRC® is a proprietary, food-q...

  6. Many-body effects in heavy fermion compounds [sic]. Final technical report for period September 1984 - January 2001

    Energy Technology Data Exchange (ETDEWEB)

    Riseborough, Peter S.

    2002-05-01

    A theoretical investigation of many-body effects in Cerium and Uranium Heavy Fermion and Mixed Valent Compounds and their experimental manifestations in thermodynamic, transport, and spectroscopic properties is discussed in this report.

  7. Algicidal and antifungal compounds from the roots of Ruta graveolens and synthesis of their analogs.

    Science.gov (United States)

    Meepagala, Kumudini M; Schrader, Kevin K; Wedge, David E; Duke, Stephen O

    2005-11-01

    Bioassay-guided fractionation of the ethyl acetate extract of Ruta graveolens roots yielded rutacridone epoxide with potent selective algicidal activity towards the 2-methyl-isoborneol (MIB)-producing blue-green alga Oscillatoria perornata, with relatively little effect on the green alga Selenastrum capricornutum. The diol-analog of rutacridone epoxide, gravacridondiol, which was also present in the same extract, had significantly less activity towards O. perornata. Rutacridone epoxide also showed significantly higher activity than commercial fungicides captan and benomyl in our micro-bioassay against the agriculturally important pathogenic fungi Colletotrichum fragariae, C. gloeosporioides, C. acutatum, and Botrytis cineara and Fusarium oxysporium. Rutacridone epoxide is reported as a direct-acting mutagen, precluding its use as an agrochemical. In order to understand the structure-activity relationships and to develop new potential biocides without toxicity and mutagenicity, some analogs containing the (2-methyloxiranyl)-dihydrobenzofuran moiety with an epoxide were synthesized and tested. None of the synthetic analogs showed comparable activities to rutacridone epoxide. The absolute stereochemistry of rutacridone was determined to be 2'(R) and that of rutacridone epoxide to be 2'(R), 3'(R) by CD and NMR analysis.

  8. Rapid and efficient synthesis of alkali metal-C[sub 60] compounds in liquid ammonia

    Energy Technology Data Exchange (ETDEWEB)

    Buffinger, D.R.; Ziebarth, R.P.; Stenger, V.A.; Recchia, C.; Pennington, C.H. (Ohio State Univ., Columbus, OH (United States))

    1993-10-06

    The reaction of stoichiometric amounts of alkali metals with C[sub 60] in liquid ammonia provides a rapid and quantitative route to M[sub x]C[sub 60] superconductors (M[sub x] = K[sub 3]/, Rb[sub 3]/, CsRb[sub 2], RbCs[sub 2], KRbCs). Annealing of the samples for 24-48 h at 375[degrees]C is required to obtain large superconducting fractions. [sup 13]C and [sup 87]Rb NMR line shapes are reported for Rb[sub 3]C[sub 60]. The [sup 13]C line shapes show the degree of rotational motion of the C[sub 60] ions varies considerably from sample to sample and is dependent on the method of preparation and subsequent heat treatment. A correlation between the degree of rotational motion and the superconducting fraction is noted and attributed to the amount of disorder in the sample. [sup 87]Rb NMR shows three peaks indicating that Rb[sub 3]C[sub 60] actually contains three different cation sites, rather than the two suggested by X-ray powder diffraction data. The third site is occupied by approximately 15% of the Rb ions in Rb[sub 3]C[sub 60] and is shown to be a subset of the tetrahedral sites in the cubic close-packed C[sub 60] lattice. Although the exact nature of the distortion required to produce the third site is unknown, it appears to be unrelated to the orientations of the C[sub 60] ions creating the site. 18 refs., 2 figs.

  9. Synthesis of nanoporous carbohydrate metal-organic framework and encapsulation of selected organic compounds

    Science.gov (United States)

    Al-Ghamdi, Saleh

    Cyclodextrin metal organic frameworks (CDMOFs) with different types of cyclodextrins (CDs) (i.e., Alpha, Beta and Gamma-CD) and coordination potassium ion sources (KOH) CDMOF-a and (C7H5KO2) CDMOF-b were synthesized and fully characterized. The physical and thermal properties of the successfully produced CDMOFs were evaluated using N2 gas sorption, thermal gravimetric analysis (TGA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The N2 gas sorption isotherm revealed high uptake into the micropores (330 cm3.g -1 for Gamma-CDMOF-a) to macropore (125 cm3.g -1 for Gamma-CDMOF-b) structures with isotherm types I and II for Gamma-CDMOFs and Alpha-CDMOFs, respectively. The Langmuir specific surface area (SSA) of Gamma-CDMOF-a (1376 m2.g-1) was significantly higher than the SSA of Alpha-CDMOF-a (289 m2.g -1) and Beta-CDMOF-a (54 m2.g-1). The TGA of dehydrated CDMOF crystals showed the structures were thermally stable up to 300 °C. The XRD of the Gamma-CDMOFs and Alpha-CDMOFs showed a highly face-centered-cubic symmetrical structure. An Aldol condensation reaction occurred during the encapsulation of acetaldehyde, hexanal, trans-2-hexenal, and ethanol into Gamma-CDMOF-a, with a SSA of 1416 m2.g -1. However, Gamma-CDMOF-b with a SSA of 499 m2.g -1 was successfully used to encapsulate acetaldehyde. The maximum release of acetaldehyde from CDMOF-b was 53 mug of acetaldehyde per g of CDMOF, which is greater than previously reported acetaldehyde encapsulation on Beta-CD inclusion complexes.

  10. Synthesis and Characterization of Two Novel Organic-Inorganic Compounds Based on Tetrahexyl and Tetraheptyl Ammonium Ions and the Preyssler Anion and Their Catalytic Activities in the Synthesis of 4-Aminopyrazolo[3,4-d]- Pyrimidines

    Directory of Open Access Journals (Sweden)

    Fatemeh Farrash Bamoharram

    2010-04-01

    Full Text Available Two novel organic–inorganic compounds based on tetrahexylammonium (THA and tetraheptylammonium (THPA ions and the Preyssler anion, [NaP5W30O110]14-, were synthesized and formulated as (THA7.7H6.3 [NaP5W30O110] (A and (THPA7.5 H6.5[N aP5W30O110] (B. The synthesized compounds were characterized by IR, UV, and TGA and used for the catalytic synthesis of 4-aminopyrazolo[3,4,-d]pyrimidine derivatives 2a-2d. Our findings showed efficient catalytic activities for A and B.

  11. Porous FeVO{sub 4} nanorods: synthesis, characterization, and gas-sensing properties toward volatile organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Kaneti, Yusuf V.; Zhang, Zhengjie; Yue, Jeffrey; Jiang, Xuchuan, E-mail: xcjiang@unsw.edu.au; Yu, Aibing [The University of New South Wales, School of Materials Science and Engineering (Australia)

    2013-09-15

    This study reports a facile hydrothermal approach for the synthesis of shape-controlled FeVO{sub 4}{center_dot}1.1H{sub 2}O nanorods and the subsequent conversion into FeVO{sub 4} nanorods upon calcination at 500 Degree-Sign C for 2 h. The lengths of the synthesized FeVO{sub 4} nanorods vary from 0.7-3.5 {mu}m, with the widths ranging from 70-270 nm. The proposed synthesis strategy does not involve the use of surfactants and requires only a very short reaction time, which is highly beneficial for the scale-up preparation. The anions of the Fe precursor are found to directly influence the shape and composition of the resultant hydrated FeVO{sub 4} products, due to the differences in their ionic strength and their abilities to intercalate into the layered structure of FeVO{sub 4}{center_dot}1.1H{sub 2}O. The Cl{sup -} ions are particularly useful in limiting the growth of the nanorods in the lateral direction without being strongly intercalated into the layered structure. The porous FeVO{sub 4} nanorods exhibit higher selectivity and sensitivity toward n-butanol compared to FeVO{sub 4} nanoparticles, due to the high surface area and porosity. The findings demonstrate for the first time the potential of nanosized FeVO{sub 4} as a sensor material for the detection of volatile gases.

  12. Synthesis and characterization of [M(III)(PS)2(L)] mixed-ligand compounds (M = Re, 99Tc; PS = phosphinothiolate; L = dithiocarbamate) as potential models for the development of new agents for SPECT imaging and radiotherapy.

    Science.gov (United States)

    Salvarese, N; Morellato, N; Venzo, A; Refosco, F; Dolmella, A; Bolzati, C

    2013-06-03

    The synthesis and characterization of a new series of neutral, six-coordinated mixed-ligand compounds [M(III)(PS)2(L)] (M = Re; (99)Tc), where PS is bis(arylalkyl)- or trialkylphosphinothiolate and L is dithiocarbamate, are reported. Stable [M(III)(PS)2(L)] complexes were easily synthesized, in good yield, starting from precursors where the metal was in different oxidation states (III, V, and VII), involving ligand-exchange and/or redox-substitution reactions. The compounds were characterized by elemental analysis, positive-ion electrospray ionization mass spectrometry, multinuclear NMR spectroscopy, cyclic voltammetry, and X-ray diffraction analysis. All complexes are constituted by the presence of the [M(III)(PS)2](+) moiety, where two phosphinothiolate ligands are tightly bound to the metal and the remaining two positions are saturated by a dithiocarbamate chelate, also carrying bulky bioactive molecules [e.g., (2-methoxyphenyl)piperazine]. X-ray analyses were performed on crystalline specimens of four different Re/(99)Tc compounds sharing a distorted trigonal-prismatic geometry, with a P2S4 coordination donor set. The possibility of easily preparing these [M(III)(PS)2(L)] complexes, starting from the corresponding permetalate anions, in mild reaction conditions and in high yield, lays the first stone to the preparation of a new series of M(III)-based (M = (99m)Tc/(188)Re) compounds potentially useful in theragnostic applications.

  13. A Case Report of Compound Odontoma Associated with an Unerupted Maxillary Central Incisor

    Directory of Open Access Journals (Sweden)

    Eda Arat Maden

    2014-02-01

    Full Text Available Odontomas generally appear as small, solitary or multiple radio-opaque lesions found on routine radiographic examinations. Traditionally, odontomas are the most common type of odontogenic tumor and they are generally asymptomatic. Occasionally, odontomas may cause disturbances in the eruption of teeth, such as impaction, delay eruption or retention of primary teeth. In general, odontomas occur more often in the permanent dentition. This is a case report of a compound composite odontoma in an 8-year-old boy, which has resulted in failure of eruption of the permanent upper right central incisor while the contra-lateral tooth had erupted. [Arch Clin Exp Surg 2014; 3(1.000: 47-51

  14. Nanoscale Synthesis and Characterization Laboratory Annual Report 2005

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V; Lesuer, D R

    2006-01-03

    The Nanoscale Synthesis and Characterization Laboratory's (NSCL) primary mission is to create and advance interdisciplinary research and development opportunities in nanoscience and technology. The initial emphasis of the NSCL has been on development of scientific solutions in support of target fabrication for the NIF laser and other stockpile stewardship experimental platforms. Particular emphasis has been placed on the design and development of innovative new materials and structures for use in these targets. Projects range from the development of new high strength nanocrystalline alloys to graded density materials to high Z nanoporous structures. The NSCL also has a mission to recruit and train personnel for Lab programs such as the National Ignition Facility (NIF), Defense and Nuclear Technologies (DNT), and Nonproliferation, Arms control and International security (NAI). The NSCL continues to attract talented scientists to the Laboratory.

  15. Fischer-Tropsch synthesis in supercritical fluids. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Akgerman, A.; Bukur, D.B.

    1998-12-31

    The objective of this study was to investigate Fischer-Tropsch Synthesis (FTS) in the supercritical phase employing a commercial precipitated iron catalysts. As the supercritical fluid the authors used propane and n-hexane. The catalyst had a nominal composition of 100 Fe/5 Cu/4.2 K/25 SiO{sub 2} on mass basis and was used in a fixed bed reactor under both normal (conventional) and supercritical conditions. Experimental data were obtained at different temperatures (235 C, 250 C, and 260 C) and synthesis gas feed compositions (H{sub 2}/CO molar feed ratio of 0.67, 1.0 and 2.0) in both modes of operation under steady state conditions. The authors compared the performance of the precipitated iron catalyst in the supercritical phase, with the data obtained in gas phase (fixed bed reactor) and slurry phase (STS reactor). Comparisons were made in terms of bulk catalyst activity and various aspects of product selectivity (e.g. lumped hydrocarbon distribution and olefin content as a function of carbon number). In order to gain better understanding of the role of intraparticle mass transfer during FTS under conventional or supercritical conditions, the authors have measured diffusivities of representative hydrocarbon products in supercritical fluids, as well as their effective diffusion rates into the pores of catalyst at the reaction conditions. They constructed a Taylor dispersion apparatus to measure diffusion coefficients of hydrocarbon products of FTS in sub and supercritical ethane, propane, and hexane. In addition, they developed a tracer response technique to measure the effective diffusivities in the catalyst pores at the same conditions. Based on these results they have developed an equation for prediction of diffusion in supercritical fluids, which is based on the rough hard sphere theory.

  16. Organic Synthesis in Ionic Liquids: Condensation of 3-Methyl-1-phenyl-5-pyrazolone with Carbonyl Compounds Catalyzed by Ethylenediammonium Diacetate(EDDA)

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    An efficient and environmental benign method is reported for the condensation of 3-methyl-1-phenyl-5-pyrazolone with carbonyl compounds in ionic liquids [Bmim]BF4 and [Bmim]PF6 catalyzed by ethylenediammonium diacetate.

  17. Evaluation of the health aspects of certain compounds found in irradiated beef. Supplement II. Possible radiolytic compounds. Final report, 1 October 1977-31 March 1979

    Energy Technology Data Exchange (ETDEWEB)

    Chinn, H.I.

    1979-03-01

    Volatile products of beef irradiated with 56 kGy (5.6 Mrad) and approximately -30 C have been identified and their health aspects discussed in a previous report. In addition to these volatile radiolytic compounds, other, nonvolatile products are possible. This report attempts to identify the compounds which might result from beef irradiation; to estimate roughly the concentrations of such products; and to evaluate their possible hazard to health. There is very little carbohydrate in beef and its radiolytic products should be relatively innocuous in the amounts produced. Few radiolytic products have been identified from the protein component of beef. The bulk of radiolytic products found in beef has come from the fat moiety. Simple triglycerides have been studied extensively and sites of bond scission have been identified. The major products are fatty acids, diglycerides, and diol diesters. The concentrations of these classes have been estimated at approximately 0.5 to 1.0 g per kg irradiated beef. Lesser amounts of many other compounds are possible, including hydrocarbons of varying chain lengths, glycerol, monoglycerides, aldehydes, and ketones. The biological effects of each of these classes have been considered.

  18. Entrepreneurship Education in the Arab States. Component II: Regional Synthesis Report

    Science.gov (United States)

    El-Kiswani, Abeer

    2013-01-01

    The UNEVOC-UNESCO International Centre in cooperation with the Regional Bureau for Education-Beirut published the regional synthesis report on Component II of the regional project on entrepreneurship education in the Arab States (2009-2012). With support from the StratREAL Foundation, the project aimed at supporting Arab countries in the…

  19. Controlled Synthesis of Polyenes by Catalytic Methods. Progress Report, December 1, 1992 -- November 30, 1993

    Science.gov (United States)

    Schrock, R. R.

    1993-12-01

    Four studies are reported: living cyclopolymerization of diethyl dipropargylmalonate by Mo(CH-t-Bu)(NAr)[OCMe(CF{sub 3}){sub 2}]{sub 2} in dimethoxyethane, effect of chain length on conductivity of polyacetylene, nonlinear optical analysis of a series of triblock copolymers containing model polyenes, and synthesis of bifunctional hexafluoro-t-butoxide Mo species and their use as initiators in ROMP reactions.

  20. Synthesis and antimicrobial activity of squalamine analogue.

    Science.gov (United States)

    Kim, H S; Choi, B S; Kwon, K C; Lee, S O; Kwak, H J; Lee, C H

    2000-08-01

    Synthesis and antimicrobial activity of squalamine analogue 2 are reported. The synthesis of 2 was accomplished from bisnoralcohol 3. The spermidine moiety was introduced via reductive amination of an appropriately functionalized 3beta-aminosterol with spermidinyl aldehyde 17 utilizing sodium triacetoxyborohydride as the reducing agent. Compound 2 shows weaker antimicrobial activity than squalamine.

  1. Synthesis gas solubility in Fischer-Tropsch slurry: Final report

    Energy Technology Data Exchange (ETDEWEB)

    Chao, K.C.; Lin, H.M.

    1988-01-01

    The objective is to investigate the phase equilibrium behavior of synthesis gases and products in a Fischer-Tropsch slurry reactor. A semi-flow apparatus has been designed and constructed for this purpose. Measurements have been made for hydrogen, cabon monoxide, methane, ethane, ethylene, and carbon dioxide in a heavy n-paraffin at temperatures from 100 to 300)degree)C and pressures 10 to 50 atm. Three n-paraffin waxes: n-eicosane (n-C/sub 20/), n-octacosane )n-C/sub 28/), and n-hexatriacontane (n-C/sub 36/), were studied to model the industrial wax. Solubility of synthesis gas mixtures of H/sub 2/ and CO in n-C/sub 28/ was also determined at two temperatures (200 and 300)degree)C) for each of three gas compositions (40.01, 50.01, and 66.64 mol%) of hydrogen). Measurements were extended to investigate the gas solubility in two industrial Fischer-Tropsch waxes: Mobilwax and SASOL wax. Observed solubility increases in the order: H/sub 2/, CO, CH/sub 4/, CO/sub 2/, C/sub 2/H/sub 4/, C/sub 2/H/sub 6/, at a given temperature pressure, and in the same solvent. Solubility increases with increasing pressure for all the gases. Lighter gases H/sub 2/ and CO show increased solubility with increasing temperature, while the heavier gases CO/sub 2/, ethane, and ethylene show decreased solubility with increasing temperature. The solubility of methane, the intermediate gas, changes little with temperature, and shows a shallow minimum at about 200)degrees)C or somewhat above. Henry's constant and partial molal volume of the gas solute at infinite dilution are determinedfrom the gas solubility data. A correlation is developed from the experimental data in the form on an equation of state. A computer program has been prepared to implement the correlation. 19 refs., 66 figs., 39 tabs.

  2. Synthesis Report on User Acceptability of Ventilation Technologies

    DEFF Research Database (Denmark)

    Larsen, Olena Kalyanova; Heiselberg, Per

    This report is prepared to summarise user satisfaction surveys available for 18 buildings in Building AdVent project. The results of user satisfaction survey are assembled in Building AdVent project D7 report for the Work Package 3. These serve a background for further discussions of acceptability...

  3. Final report on CCQM-K47: Volatile organic compounds in methanol

    Science.gov (United States)

    Pérez Urquiza, Melina; Maldonado Torres, Mauricio; Mitani, Yoshito; Schantz, Michele M.; Duewer, David L.; May, Wille E.; Parris, Reenie M.; Wise, Stephen A.; Kaminski, Katja; Philipp, Rosemarie; Win, Tin; Rosso, Adriana; Kim, Dal Ho; Ishikawa, Keiichiro; Krylov, A. I.; Kustikov, Y. A.; Baldan, Annarita

    2013-01-01

    At the October 2005 CCQM Organic Analysis Working Group Meeting (IRMM, Belgium), the decision was made to proceed with a Key Comparison study (CCQM-K47) addressing the calibration function for the determination of volatile organic compounds (VOCs) used for water quality monitoring. This was coordinated by CENAM and NIST. Benzene, o-xylene, m-xylene and p-xylene were chosen as representative VOCs. The solvent of choice was methanol. Key Comparison CCQM-K47 demonstrated the capabilities of participating NMIs to identify and measure the four target VOCs in a calibration solution using GC-based methods. The measurement challenges in CCQM-K47, such as avoiding volatility loss, achieving adequate chromatographic resolution and isolating potential interferences, are typical of those required for value-assigning volatile reference materials. Participants achieving comparable measurements for all four VOCs in this Key Comparison should be capable of providing reference materials and measurements for VOCs in solutions when present at concentration levels greater than 10 µg/g. Main text. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

  4. A critical review of reported air concentrations of organic compounds in aircraft cabins.

    Science.gov (United States)

    Nagda, N L; Rector, H E

    2003-09-01

    This paper presents a review and assessment of aircraft cabin air quality studies with measured levels of volatile and semivolatile organic compounds (VOCs and SVOCs). VOC and SVOC concentrations reported for aircraft cabins are compared with those reported for residential and office buildings and for passenger compartments of other types of transportation. An assessment of measurement technologies and quality assurance procedures is included. The six studies reviewed in the paper range in coverage from two to about 30 flights per study. None of the monitored flights included any unusual or episodic events that could affect cabin air quality. Most studies have used scientifically sound methods for measurements. Study results indicate that under routine aircraft operations, contaminant levels in aircraft cabins are similar to those in residential and office buildings, with two exceptions: (1). levels of ethanol and acetone, indicators of bioeffluents and chemicals from consumer products are higher in aircraft than in home or office environments, and (2). levels of certain chlorinated hydrocarbons and fuel-related contaminants are higher in residential/office buildings than in aircraft. Similarly, ethanol and acetone levels are higher in aircraft than in other transportation modes but the levels of some pollutants, such as m-/p-xylenes, tend to be lower in aircraft.

  5. [Infantile hypophosphatasia caused by a novel compound heterozygous mutation: a case report and pedigree analysis].

    Science.gov (United States)

    Li, Deng-Feng; Lan, Dan; Zhong, Jing-Zi; Dewan, Roma Kajal; Xie, Yan-Shu; Yang, Ying

    2017-05-01

    This article reported the clinical features of one child with infantile hypophosphatasia (HPP) and his pedigree information. The proband was a 5-month-old boy with multiple skeletal dysplasia (koilosternia, bending deformity of both radii, and knock-knee deformity of both knees), feeding difficulty, reduction in body weight, developmental delay, recurrent pneumonia and respiratory failure, and a significant reduction in blood alkaline phosphatase. Among his parents, sister, uncle, and aunt (other family members did not cooperate with us in the examination), his parents and aunt had a slight reduction in alkaline phosphatase and his aunt had scoliosis; there were no other clinical phenotypes or abnormal laboratory testing results. His ALPL gene mutation came from c.228delG mutation in his mother and c.407G>A compound heterozygous mutation in his father. His aunt carried c.228delG mutation. The c.407G>A mutation had been reported as the pathogenic mutation of HPP, and c.228delG mutation was a novel pathogenic mutation. Hypophosphatasia is caused by ALPL gene mutation, and ALPL gene detection is an effective diagnostic method. This study expands the mutation spectrum of ALPL gene and provides a theoretical basis for genetic diagnosis of this disease.

  6. Biological upgrading of coal-derived synthesis gas: Final report

    Energy Technology Data Exchange (ETDEWEB)

    Barik, S.; Johnson, E.R.; Ko, C.W.; Clausen, E.C.; Gaddy, J.L.

    1986-10-01

    The technical feasibility of the biological conversion of coal synthesis gas to methane has been demonstrated in the University of Arkansas laboratories. Cultures of microorganisms have been developed which achieve total conversion in the water gas shift and methanation reactions in either mixed or pure cultures. These cultures carry out these conversions at ordinary temperatures and pressures, without sulfur toxicity. Several microorganisms have been identified as having commercial potential for producing methane. These include a mixed culture of unidentified bacteria; P. productus which produces acetate, a methane precursor; and Methanothrix sp., which produces methane from acetate. These cultures have been used in mixed reactors and immobilized cell reactors to achieve total CO and H/sub 2/ conversion in a retention time of less than two hours, quite good for a biological reactor. Preliminary economic projections indicate that a biological methanation plant with a size of 5 x 10/sup 10/ Btu/day can be economically attractive. 42 refs., 26 figs., 86 tabs.

  7. Synthesis gas demonstration plant program, Phase I. Site confirmation report

    Energy Technology Data Exchange (ETDEWEB)

    1978-12-01

    With few reservations, the Baskett, Kentucky site exhibits the necessary characteristics to suggest compatibility with the proposed Synthesis Gas Demonstration Plant Project. An evaluation of a broad range of technical disciplinary criteria in consideration of presently available information indicated generally favorable conditions or, at least, conditions which could be feasibly accommodated in project design. The proximity of the Baskett site to market areas and sources of raw materials as well as a variety of transportation facilities suggests an overall favorable impact on Project economic feasibility. Two aspects of environmental engineering, however, have been identified as areas where the completion or continuation of current studies are required before removing all conditions on site suitability. The first aspect involves the current contradictory status of existing land use and planning ordinances in the site area. Additional investigation of the legality of, and local attitudes toward, these present plans is warranted. Secondly, terrestrial and aquatic surveys of plant and animal life species in the site area must be completed on a seasonal basis to confirm the preliminary conclusion that no exclusionary conditions exist.

  8. Standards for reporting qualitative research: a synthesis of recommendations.

    Science.gov (United States)

    O'Brien, Bridget C; Harris, Ilene B; Beckman, Thomas J; Reed, Darcy A; Cook, David A

    2014-09-01

    Standards for reporting exist for many types of quantitative research, but currently none exist for the broad spectrum of qualitative research. The purpose of the present study was to formulate and define standards for reporting qualitative research while preserving the requisite flexibility to accommodate various paradigms, approaches, and methods. The authors identified guidelines, reporting standards, and critical appraisal criteria for qualitative research by searching PubMed, Web of Science, and Google through July 2013; reviewing the reference lists of retrieved sources; and contacting experts. Specifically, two authors reviewed a sample of sources to generate an initial set of items that were potentially important in reporting qualitative research. Through an iterative process of reviewing sources, modifying the set of items, and coding all sources for items, the authors prepared a near-final list of items and descriptions and sent this list to five external reviewers for feedback. The final items and descriptions included in the reporting standards reflect this feedback. The Standards for Reporting Qualitative Research (SRQR) consists of 21 items. The authors define and explain key elements of each item and provide examples from recently published articles to illustrate ways in which the standards can be met. The SRQR aims to improve the transparency of all aspects of qualitative research by providing clear standards for reporting qualitative research. These standards will assist authors during manuscript preparation, editors and reviewers in evaluating a manuscript for potential publication, and readers when critically appraising, applying, and synthesizing study findings.

  9. Insights into Stabilization of the 99TcVO Core for Synthesis of 99TcVO Compounds

    Energy Technology Data Exchange (ETDEWEB)

    McGregor, Donna; Burton-Pye, Benjamin P.; Lukens, Wayne W.; Howell, Robertha C.; Francesconi, Lynn C.

    2014-01-01

    Synthesis of technetium-99 (99Tc; t1/2: 2.1 105 years, max: 253 keV) materials is of importance in studies of the nuclear fuel cycle where Tc is a major fission product (6percent thermal yield from 235U and 239Pu), in understanding radioactive tank waste composition, and in identifying 99mTc compounds for nuclear medicine imaging. One of the most useful synthetic starting materials, (NBu4)TcOCl4, is susceptible to disproportionation in water to form TcO4 and TcIV species, especially TcO2 2H2O. This unwanted reaction is especially problematic when working with ligands bearing hard donor atoms, such as oxygen, where the stability with the soft TcV=O3+ core may be low. Polyoxometalates (POMs) are such ligands. They possess defect sites with four hard oxygen atoms and show low (ca. 108) stability constants with transition metals. Tc complexes of POMs are molecular-level models for Tc metal oxide solid-state materials and can provide information on coordination and redox environments of metal oxides that stabilize low-valent Tc. In order to synthesize pure Tc POM complexes [TcVO(1-P2W17O61)]7 (TcVO-1) and [TcVO(2-P2W17O61)]7 (TcVO-2) from (NBu4)TcOCl4, we have identified strategies that minimize formation of TcIV species and optimize the formation of pure TcV species. The parameters that we consider are the amount of ethylene glycol, which is employed as a transfer ligand to prevent hydrolysis of (NBu4)TcOCl4, and the precipitating agent. The TcIV species that contaminates the non-optimized syntheses is likely a TcIV -oxido-bridged dimer [TcIV-(-O)2-TcIV]. We also employ a novel procedure where the 2 ligand is photoactivated and reduced (in the presence of a sacrificial electron donor) to subsequently reduce TcVIIO4 to an isolatable TcVO-2 product that is remarkably free of TcIV.

  10. Synthesis by plasma and characterization of compounds derived from polyacetylene; Sintesis por plasma y caracterizacion de compuestos derivados del poliacetileno

    Energy Technology Data Exchange (ETDEWEB)

    Vasquez O, M

    2004-07-01

    This work presents a study on, the synthesis by plasma and the characterization of an aliphatic conjugated polymer, polyacetylene-chlorinated (Pac), and two aromatic polymers, Poly pyrrole (P Py-Cl) and Poly thiophene (Pth-Cl) synthesized with chlorine and the electrical conductivity. The last two polymers were synthesized to compare the chlorine-polymer interaction in aliphatic and aromatic polymers synthesized by plasma and their repercussion on the electrical transport of charges in the material. The structure and morphology of the polymers were studied using scanning electron microscopy (Sem), energy dispersive spectroscopy (EDS), infrared spectroscopy (Ft-IR), conductivity analysis and X-Ray photon spectroscopy (XPS). The results showed that Pac is soluble in acetone and other organic solvents, which indicates a low proportion of crosslinking in the polymers. This point is important because the crosslinking reduces the electrical conductivity in the material. The Pac conductivity is in the range of 1 x 10{sup -12} to 6 x 10{sup -4} S/cm in the internal of 35- 90% of relative humidity. A possible mechanism for the transport of electrical charges in Pac is by means of the double and simple conjugated bonds in the polymers. Pth-Cl and P Py-Cl present electric conductivity in the interval of 9 x 10{sup -5} to 1 x 10{sup -2} S/cm and show a great dependence on the relative humidity. The chlorine addition in these polymers was through simultaneous polymerization with chloroform. This last compound can decompose if the energy of the plasma is relatively high, and the fragments can link to the polymer in a hybrid process of copolymerization. An important point of this work is that the polymer is soluble, a difference of the obtained via plasma as the poli aniline, P Py-CI and Pth-Cl both studied in this work. If took in account that the Pac is single the monomer and that P Py-Cl and Pth-CI is affected by the chlorine that modifies the conductivity of the material

  11. Final Report on XStack: Software Synthesis for High Productivity ExaScale Computing

    Energy Technology Data Exchange (ETDEWEB)

    Solar-Lezama, Armando [Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States). Computer Science and Artificial Intelligence Lab.

    2016-07-12

    The goal of the project was to develop a programming model that would significantly improve productivity in the high-performance computing domain by bringing together three components: a) Automated equivalence checking, b) Sketch-based program synthesis, and c) Autotuning. The report provides an executive summary of the research accomplished through this project. At the end of the report is appended a paper that describes in more detail the key technical accomplishments from this project, and which was published in SC 2014.

  12. Synthesis, structures of four coordination compounds constructed from o-methacrylamidobenzoic acid and their relationship between structure and solid state luminescence

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Hong-Xia; Ma, Yong; Zhou, Feng; Wu, Bing [Key Laboratory of Organic Synthesis of Jiangsu Province, School of Chemistry, Chemical Engineering and Materials Science, Soochow University(DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China); Key Laboratory of Energy-Saving And Environmental Protection Materials Test and Technical Service Center of Jiangsu Province, Soochow University (DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China); Xu, Qing-Feng, E-mail: xuqingfeng@suda.edu.cn [Key Laboratory of Organic Synthesis of Jiangsu Province, School of Chemistry, Chemical Engineering and Materials Science, Soochow University(DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China); Key Laboratory of Energy-Saving And Environmental Protection Materials Test and Technical Service Center of Jiangsu Province, Soochow University (DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China); Lu, Jian-Mei, E-mail: lujm@suda.edu.cn [Key Laboratory of Organic Synthesis of Jiangsu Province, School of Chemistry, Chemical Engineering and Materials Science, Soochow University(DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China); Key Laboratory of Energy-Saving And Environmental Protection Materials Test and Technical Service Center of Jiangsu Province, Soochow University (DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China); Ge, Jian-Feng [Key Laboratory of Organic Synthesis of Jiangsu Province, School of Chemistry, Chemical Engineering and Materials Science, Soochow University(DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China); Key Laboratory of Energy-Saving And Environmental Protection Materials Test and Technical Service Center of Jiangsu Province, Soochow University (DuShuHu Campus), 199 Renai Road, Suzhou, 215123 (China)

    2013-07-15

    Four new coordination compounds, namely, Zn(o-MAABA){sub 2}(Phen) (1), [Cd(o-MAABA){sub 2}·2H{sub 2}O]{sub 2} (2), ([Pb{sub 2}Cl{sub 2}(o-MAABA){sub 2}(Phen){sub 4}])·2H{sub 2}O (3·2H{sub 2}O), [Pb(NO{sub 3})(o-MAABA)(Phen)]{sub n} (4), where o-MAABA=o-methacrylamidobenzoic acid and phen=1, 10-phenanthroline, have been synthesized. All compounds were fully confirmed by FT-IR, elemental analysis and TGA analysis. Their structures were determined by single crystal X-ray diffraction, in which compound 1 shows a mononuclear structure, compounds 2 and 3 have binuclear structures and compound 4 shows an infinite chain. In 2 and 4, the adjacent chains are extended into a 3D supramolecular architecture via π–π interactions. Solid-state room temperature luminescence spectra revealed that emission bands of compound 1 were located at 524 nm (λ{sub ex}=352 nm) and compound 4 at 479 and 584 nm (λ{sub ex}=390 nm) assigned to the excimer formation. The emission at 454 nm (λ{sub ex}=340 nm) of compound 2 was mainly ascribed to the Ligand–Metal Charge Transfer (LMCT). - Graphical abstract: Four coordination compounds constructed by o-methacrylamidobenzoic, phenanthroline and metal ions are reported. The photoluminescent properties is studied, which is affected by the molecular stacking and LMCT.

  13. Alternative fuels and chemicals from synthesis gas. Quarterly report, April 1--June 30, 1995

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1995-12-31

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE`s LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts. The paper reports the progress on the following tasks: engineering and modifications: AFDU shakedown, operations, deactivation and disposal; and research and development on new processes for DME, chemistry and catalyst development, and oxygenates via synthesis gas.

  14. A dinuclear end-on azide-bridged copper(II) compound with weak antiferromagnetic interaction - Synthesis, characterization, magnetism and X-ray structure of bis[(μ-azido-κN1)-(azido-κN1)(1,3-bis(benzimidazol-2-yl)-2-methylpropane)copper(II)

    Science.gov (United States)

    van Albada, Gerard A.; Mutikainen, Ilpo; Roubeau, Olivier; Reedijk, Jan

    2013-03-01

    The centrosymmetric dinuclear compound of formula [Cu(μ-N3-κN1)(N3-κN1)(bbmp)]2 is reported. Synthesis, characterization, physical properties are determined in detail, together with its 3D structure. The dinuclear end-on azide-bridged copper(II) compound displays a weak antiferromagnetic interaction, despite the fact that the magnetic orbitals overlap. The Cu-Cu contact distance is 3.1867(8) Å, while the Cu-Nazide-Cu angle is 103.41(14)°. The IR spectra of the azido ligands are as expected for such coordinated azides.

  15. Synthesis and Properties of Dimesogenic Compounds Containing Cholesterol and 4-(trans-4-n-Alkylcyclohexyl)- benzoic Acid Moieties

    Institute of Scientific and Technical Information of China (English)

    YU, Haibo; HOU, Ruibin; CHEN, Tie; YIN, Bingzhu; MUHAMMAD, Jamil; JEON, Youngja

    2009-01-01

    A series of novel dimesogenic compounds containing cholesterol and 4-(trans-4-n-alkylcyclohexyl)benzoic acid moieties were synthesized. The two mesogenic units of these compounds are linked with ω-oxyalkanoyl spacers of varying lengths. The chemical structure and mesomorphic properties of this series of compounds were characterized by FT-IR, MS, 1H NMR, polarizing optical microscopy (POM) and DSC techniques. The average viscosity and helical twisting power (HTP) in host liquid crystals of selected dimesogenic compounds were also measured. It was found that most of the present novel series of compounds exhibited only cholesteric mesophase with lower phase transition temperatures, and the average viscosity and HTP of selected compounds were similar to or superior to cholesteryl nonylate.

  16. Synthesis and Structure of Supramolecular Compound with Ethyl 2-(4-Aminophenoxy)acetate Based on 18-Crown-6%Synthesis and Structure of Supramolecular Compound with Ethyl 2-(4-Aminophenoxy)acetate Based on 18-Crown-6

    Institute of Scientific and Technical Information of China (English)

    王文祥; 孙素文; 熊仁根

    2012-01-01

    The title ammonium compound ethyl 2-(4-aminophenoxy)acetate (C10 H13NO3, I) and its crown ether inclusion complex {[(CIoHI4NO3)·(18-crown-6)]·[PF6] , II} (18-crown-6 = 1,4,7,10,13,16-hexaoxacyclo-octadecane) were synthesized. The ammonium compound I was determined by 11-t NMR, IR and ESI-MS techiniques. X-ray crystal- lography reveals that compound I crystallizes in the triclinic system with space group of P-l, all the atoms in | are almost coplanar except H, and N--H…O hydrogen bonds lead to the formation of one dimensional chain. The ro- tator-stator-like compound 11 was crystallizes in the centrosymmetric monoclinic system with space group of P21/c. The supramolecular was formed via N--H…O hydrogen-bond interactions. Temperature-dependent dielectric constants of compound II were measured.

  17. Two novel compound heterozygous BMP1 mutations in a patient with osteogenesis imperfecta: a case report.

    Science.gov (United States)

    Sangsin, Apiruk; Kuptanon, Chulaluck; Srichomthong, Chalurmpon; Pongpanich, Monnat; Suphapeetiporn, Kanya; Shotelersuk, Vorasuk

    2017-03-04

    Osteogenesis imperfecta (OI) is a collagen-related bone dysplasia leading to a susceptibility to fractures. OI can be caused by mutations in several genes including BMP1. It encodes two isoforms, bone morphogenetic protein 1 (BMP1) and mammalian tolloid (mTLD); both have proteolytic activity to remove the C-propeptide from procollagen. We report a Thai OI patient who had his first fracture at the age of three months. Using next generation sequencing, we successfully identified two novel compound heterozygous BMP1 mutations. One mutation, c.796_797delTT (p.Phe266Argfs*25) affects both BMP1 and mTLD isoforms, while the other, c.2108-2A > G, affects only the BMP1 isoform. Preservation of the mTLD may explain the relatively less severe clinical phenotype in this patient. Intravenous bisphosphonate was given from the age of 8 months to 5 years. He was free from fractures for 9 months before discontinuation. This case expands the mutation spectrum of BMP1, strengthens the correlation between genotype and phenotype, and supports the benefits of bisphosphonate in OI patients with BMP1 mutations.

  18. Synthesis of deuterium-labelled compounds for FOTEK project; Syntese af deuterium-maerkede forbindelser til FOeTEK projektet

    Energy Technology Data Exchange (ETDEWEB)

    Joergensen, O.; Egsgaard, H.; Larsen, E. [Forskningscenter Risoe, Roskilde (Denmark)

    1996-06-01

    In the FoTech project there have been utilized labelled compounds of stable isotopes as internal standards. Some of these compounds are commercially available ({sup 13}C-labelled PCB congeners, {sup 13}C-labelled diethylstilbestrol for determination of anabolic steroids). Others, like D{sub 9}-clenbuterol, D{sub 3}-clenbuterol, D{sub 3}-zeramol and D{sub 3}-dimetridazol have been synthesized. General aspects of deuterium compounds labelling are considered. (EG).

  19. Recent development in synthesis and application of amine compounds%胺类化合物合成与应用研究进展

    Institute of Scientific and Technical Information of China (English)

    牛亚男; 钟宏; 王帅; 马鑫

    2014-01-01

    The synthesis methods of amine compounds according to the various hydrocarbon groups,espe-cially the aliphatic amines and aromatic amines are reviewed. The applications in the fields of flotation, metallurgy and wastewater treatment are also introduced. Based on the review,the future research of amine compounds is presented.%主要依照烃基的不同,分类介绍胺类化合物的合成研究现状,详述了脂肪胺、芳香胺的合成。阐述了胺类化合物在矿物浮选、湿法冶金及废水处理等工业应用的进展,并由此提出胺类化合物未来研究的发展趋势。

  20. SYNTHESIS OF p-METHOXY-CYNNAMIL- p-METOXYCINAMATE FROM ETHYL p-METHOXYCINAMAT WAS ISOLATED FROM DRIED RHIZOME Kaempferia Galanga L AS SUNSCREEN COMPOUND

    Directory of Open Access Journals (Sweden)

    Titik Taufikkurohmah

    2010-06-01

    Full Text Available Synthesis of p-methoxy-cynnamil-p-methoxy-cinnamate, (PMS2O from ethyl-p-methoxy-cinnamate (EPMS from dry rhizome of kaempferia galanga L as sunscreen compound have been done. Isolation of EPMS was done by percholation using ethanol 96 % and recrystallitation using methanol to have 2.2 % yield. Hydrolysis of EPMS using alcoholic KOH resulted methoxycinnamic acid (APMS of 90.26 % yield. Reduction EPMS using lithium aluminium hydride in dry ether would give p-methoxycinnamoyl alcohol (PMS-OH of 41.98 % yield. Then reaction of p-methoxycinnamoyl chloride (PMS-Cl and PMS-OH in chloroform would produce p-methoxycinnamoyl p-methoxycinnamate ((PMS2O of 1.77 % yield. All compound were identified by TLC and several spectrometry methodes i.e. U.V Vis, IR, 1H-NMR and GC-MS   Keywords: esther cinnamate, sunscreen, Kaempferia galanga.

  1. Advances in String Theory in Curved Backgrounds A Synthesis Report

    CERN Document Server

    Sánchez, N G

    2003-01-01

    A synthetic report of the advances in the study of classical and quantum string dynamics in curved backgrounds is provided, namely: the new feature of multistring solutions; the effect of a cosmological constant and of spacial curvature on classical and quantum strings; classical splitting of fundamental strings;the general string evolution in constant curvature spacetimes;the conformal invariant effects;strings on plane waves, shock waves and spacetime singularities and its spectrum. New developments in string gravity and string cosmology are reported: string driven cosmology and its predictions;the primordial gravitation wave background; non-singular string cosmologies from exact conformal field theories;QFT, string temperature and the string phase of de Sitter space; the string phase of black holes;new dual relation between QFT regimes and string regimes and the 'QFT/String Tango'; new coherent string states and minimal uncertainty principle in string theory

  2. Polybenzimidazole compounds

    Science.gov (United States)

    Klaehn, John R.; Peterson, Eric S.; Wertsching, Alan K.; Orme, Christopher J.; Luther, Thomas A.; Jones, Michael G.

    2010-08-10

    A PBI compound that includes imidazole nitrogens, at least a portion of which are substituted with an organic-inorganic hybrid moiety. At least 85% of the imidazole nitrogens may be substituted. The organic-inorganic hybrid moiety may be an organosilane moiety, for example, (R)Me.sub.2SiCH.sub.2--, where R is selected from among methyl, phenyl, vinyl, and allyl. The PBI compound may exhibit similar thermal properties in comparison to the unsubstituted PBI. The PBI compound may exhibit a solubility in an organic solvent greater than the solubility of the unsubstituted PBI. The PBI compound may be included in separatory media. A substituted PBI synthesis method may include providing a parent PBI in a less than 5 wt % solvent solution. Substituting may occur at about room temperature and/or at about atmospheric pressure. Substituting may use at least five equivalents in relation to the imidazole nitrogens to be substituted or, preferably, about fifteen equivalents.

  3. Improved synthesis of glycine, taurine and sulfate conjugated bile acids as reference compounds and internal standards for ESI-MS/MS urinary profiling of inborn errors of bile acid synthesis.

    Science.gov (United States)

    Donazzolo, Elena; Gucciardi, Antonina; Mazzier, Daniela; Peggion, Cristina; Pirillo, Paola; Naturale, Mauro; Moretto, Alessandro; Giordano, Giuseppe

    2017-04-01

    Bile acid synthesis defects are rare genetic disorders characterized by a failure to produce normal bile acids (BAs), and by an accumulation of unusual and intermediary cholanoids. Measurements of cholanoids in urine samples by mass spectrometry are a gold standard for the diagnosis of these diseases. In this work improved methods for the chemical synthesis of 30 BAs conjugated with glycine, taurine and sulfate were developed. Diethyl phosphorocyanidate (DEPC) and diphenyl phosphoryl azide (DPPA) were used as coupling reagents for glycine and taurine conjugation. Sulfated BAs were obtained by sulfur trioxide-triethylamine complex (SO3-TEA) as sulfating agent and thereafter conjugated with glycine and taurine. All products were characterized by NMR, IR spectroscopy and high resolution mass spectrometry (HRMS). The use of these compounds as internal standards allows an improved accuracy of both identification and quantification of urinary bile acids. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Advances in Synthesis and Application of Metal Phthalocyanine Compounds%酞菁金属化合物的合成与应用进展

    Institute of Scientific and Technical Information of China (English)

    程振华; 蔡婷婷; 陈际海; 周文博; 刘咸尚; 夏道宏

    2012-01-01

    综述了主要涉及铁、钴、镍、铜和锌等过渡金属元素的酞菁金属化合物的研究进展.在单核酞菁金属合成的基础上,目前主要研究双核及多核酞菁金属的合成方法.在酞菁金属的芳环上引人种类不同、数目不同的各种取代基,能大大改善酞菁金属化合物的物理及化学性能,为酞菁金属新材料的应用提供基础.开发酞菁金属化合物的绿色化学合成路线是今后的发展方向.%Research progresses in synthesis and application of metal phthalocyanine compounds, which mainly includes transition metals, namely Fe, Co, Ni, Cu and Zn, are introduced. The synthesis methods for dinuclear and polynuclear metal phthalocyanine compounds caught more attention now than that for uninuclear one. It is demonstrated that by the introduction of different kinds and different number of substituent groups to the aromatic rings of phthalocyanines, the physical and chemical properties of the metal phthalocyanine compounds are greatly changed, which is more favorable to the application of these new materials. The review points out that the development of the metal phthalocyanine compounds is trending towards green synthetic routes.

  5. Compound odontoma causing airway obstruction of the newborn: a case report.

    Science.gov (United States)

    Tam, D; Francis, L; Perry, C; Thirwall, A

    2006-10-01

    A newborn presented with acute airway obstruction secondary to a compound odontoma of the hard palate/nasal floor. This is the first case recorded in the literature. We review the pathology of compound odontomas and discuss the management of this rare and interesting case.

  6. On Revising Noun Compounds: Four Tests. CDC Technical Report No. 5.

    Science.gov (United States)

    Kaufer, David S.; Steinberg, Erwin R.

    Many influential style guides endorse the stylistic prescription that writers, particularly technical writers, should revise noun compounds into phrasal or clausal paraphrases. While the prescription is well-intentioned, it fails to take into account that a reader's comprehension of compounds, whether long or short, is a complex process dependent…

  7. Design and synthesis of reactive separation systems. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Doherty, M.F.

    1992-12-31

    During the last decade there has been a rapid upturn in interest in reactive distillation. The chemical process industry recognizes the favorable economics of carrying out reaction simultaneously with distillation for certain classes of reacting systems, and many new processes have been built based on this technology. Interest is also increasing by academics and software vendors. Systematic design methods for reactive distillation systems have only recently begun to emerge. In this report we survey the available design techniques and point out the contributions made by our group at the University of Massachusetts.

  8. Hydroxylation activity of P450 BM-3 mutant F87V towards aromatic compounds and its application to the synthesis of hydroquinone derivatives from phenolic compounds.

    Science.gov (United States)

    Sulistyaningdyah, Woro Triarsi; Ogawa, Jun; Li, Qing-Shan; Maeda, Chiharu; Yano, Yuki; Schmid, Rolf D; Shimizu, Sakayu

    2005-06-01

    Cytochrome P450 BM-3 from Bacillus megaterium is a fatty acid hydroxylase exhibiting selectivity for long-chain substrates (12-20 carbons). Replacement of Phe87 in P450 BM-3 by Val (F87V) greatly increased its activity towards a variety of aromatic and phenolic compounds. The apparent initial reaction rates of F87V as to benzothiophene, indan, 2,6-dichlorophenol, and 2-(benzyloxy)phenol were 227, 204, 129, and 385 nmol min(-1) nmol(-1) P450, which are 220-, 66-, 99-, and 963-fold those of the wild type, respectively. These results indicate that Phe87 plays a critical role in the control of the substrate specificity of P450 BM-3. Furthermore, F87V catalyzed regioselective hydroxylation at the para position of various phenolic compounds. In particular, F87V showed high activity as to the hydroxylation of 2-(benzyloxy)phenol to 2-(benzyloxy)hydroquinone. With F87V as the catalyst, 0.71 mg ml(-1) 2-(benzyloxy)hydroquinone was produced from 1.0 mg ml(-1) 2-(benzyloxy)phenol in 4 h, with a molar yield of 66%.

  9. USING OF Agrobacterium-MEDIATED TRANSFORMATION FOR THE BIOTECHNOLOGICAL IMPROVEMENT OF COMPOSITAE PLANTS. ІІ. SYNTHESIS OF BIOACTIVE COMPOUNDS IN TRANSGENIC PLANTS AND «HAIRY» ROOTS

    Directory of Open Access Journals (Sweden)

    N. A. Matvieieva

    2015-04-01

    Full Text Available The review focused on the data concerning current state in the field of Compositae “hairy” roots and transgenic plants construction using A.tumefaciens- and A. rhizogenes-mediated transformation to obtain biologically active compounds, including recombinant proteins. The article presents data on the results of genetic transformation of Cichorium intybus, Lactuca sativa, Artemisia annua, Artemisia vulgaris, Calendula officinalis, Withania somnifera and other Compositae plants as well as studies on the artemisinin, flavonoids, polyphenols, fructans and other compounds accumulation in transgenic plants and roots. The data show that the use of biotechnological approaches for construction of "hairy" roots and transgenic plants with new features are of great interest. The possibility of increase in the accumulation of naturally synthesized bioactive compounds and recombinant proteins production via A. tumefaciens and A. rhizogenes-mediated transformation have been shown. In vitro cultivation of transgenic plants characterized by high level of bioactive compounds accumulation and synthesis of recombinant proteins makes it possible to obtain guaranteed pure raw material. Using of biotechnological approaches preserved natural populations of plants is particularly important for rare and endangered plant species.

  10. Prebiotic Synthesis of Methionine and Other Sulfur-Containing Organic Compounds on the Primitive Earth: A Contemporary Reassessment Based on an Unpublished 1958 Stanley Miller Experiment

    Science.gov (United States)

    Parker, Eric T.; Cleaves, H. James; Callahan, Michael P.; Dworkin, Jason P.; Glavin, Daniel P.; Lazcano, Antonio

    2010-01-01

    Original extracts from an unpublished 1958 experiment conducted by the late Stanley L. Miller were recently found and analyzed using modern state-of-the-art analytical methods. The extracts were produced by the action of an electric discharge on a mixture of methane (CH4), hydrogen sulfide (H2S), ammonia (NH3), and carbon dioxide (CO2). Racemic methionine was farmed in significant yields, together with other sulfur-bearing organic compounds. The formation of methionine and other compounds from a model prebiotic atmosphere that contained H2S suggests that this type of synthesis is robust under reducing conditions, which may have existed either in the global primitive atmosphere or in localized volcanic environments on the early Earth. The presence of a wide array of sulfur-containing organic compounds produced by the decomposition of methionine and cysteine indicates that in addition to abiotic synthetic processes, degradation of organic compounds on the primordial Earth could have been important in diversifying the inventory of molecules of biochemical significance not readily formed from other abiotic reactions, or derived from extraterrestrial delivery.

  11. Synthesis, spectroscopic characterization and crystallographic behavior of a biologically relevant novel indole-fused heterocyclic compound - Experimental and theoretical (DFT) studies

    Science.gov (United States)

    Sharma, Sakshi; Brahmachari, Goutam; Banerjee, Bubun; Nurjamal, Khondekar; Kumar, Abhishek; Srivastava, Ambrish Kumar; Misra, Neeraj; Pandey, Sarvesh Kumar; Rajnikant; Gupta, Vivek K.

    2016-08-01

    The present communication deals with the eco-friendly synthesis, spectral properties and X-ray crystal structure of an indole derivative - Ethyl 2'-amino-3'-cyano-6'-methyl-5-nitro-2-oxospiro [indoline-3,4'-pyran]-5'-carboxylate. The title compound was synthesized in 87% yield. The crystal structure of the molecule is stabilized by intermolecular Nsbnd H … N, Nsbnd H … O and Csbnd H … π interactions. The molecule is organized in the crystal lattice forming sheet like structure. To interpret the experimental data, ab initio computations of the vibrational frequencies were carried out using the Gaussian 09 program followed by the full optimizations done using Density Functional Theory (DFT) at B3LYP/6-31 + G(d,p) level. The combined use of experiments and computations allowed a firm assignment of the majority of observed bands for the compound. The calculated highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) with frontier orbital gap were presented. The electronic and charge transfer properties have been explained on the basis of highest occupied molecular orbitals (HOMOs), lowest unoccupied molecular orbitals (LUMOs) and density of states (DOS). From the optimized geometry of the molecule, molecular electrostatic potential (MEP) distribution, frontier molecular orbitals (FMOs) of the title compound have been calculated in the ground state theoretically. The theoretical results showed good agreement with the experimental values. First hyperpolarizability values have been calculated to describe the nonlinear optical (NLO) property of the synthesized compound.

  12. Development of pharmaceuticals with radioactive rhenium for cancer therapy. Production of {sup 186}Re and {sup 188}Re, synthesis of labeled compounds and their biodistributions

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-03-01

    Production of the radioactive rhenium isotopes {sup 186}Re and {sup 188}Re, and synthesis of their labeled compounds have been studied together with the biodistributions of the compounds. This work was carried out by the Working Group on Radioactive Rhenium, consisting of researchers of JAERI and some universities, in the Subcommittee for Production and Radiolabeling under the Consultative Committee of Research on Radioisotopes. For {sup 186}Re, production methods by the {sup 185}Re(n,{gamma}){sup 186}Re reaction in a reactor and by the {sup 186}W(p,n){sup 186}Re reaction with an accelerator, which can produce nocarrier-added {sup 186}Re, have been established. For {sup 188}Re, a production method by the double neutron capture reaction of {sup 186}W, which produces a {sup 188}W/{sup 188}Re generator, has been established. For labeling of bisphosphonate, DMSA, DTPA, DADS, aminomethylenephosphonate and some monoclonal antibodies with the radioactive rhenium isotopes, the optimum conditions, including pH, the amounts of reagents and so on, have been determined for each compound. The biodistributions of each of the labeled compounds in mice have been also obtained. (author)

  13. A New Type of NADH Model Compound: Synthesis and Enantioselective Reduction of Benzoylformates to the Corresponding Mandelates

    Directory of Open Access Journals (Sweden)

    Xin-Liang Tang

    2007-05-01

    Full Text Available A new type of NADH model compound with good reactivity and enantioselectivity has been synthesized in good yields by an efficient and convenient synthetic method. The structures of these model compounds were confirmed by 1H and 13C-NMR and MS.

  14. Synthesis of new 1,2,4-triazole compounds containing Schiff and Mannich bases (morpholine) with antioxidant and antimicrobial activities.

    Science.gov (United States)

    Ünver, Yasemin; Deniz, Sadik; Çelik, Fatih; Akar, Zeynep; Küçük, Murat; Sancak, Kemal

    2016-01-01

    Compound 2 was synthesized by reacting CS2/KOH with compound 1. The treatment of compound 2 with hydrazine hydrate produced compound 3. Then, compound 3 was converted to Schiff bases (4a-d) by the handling with several aromatic aldehydes. The treatment of triazole compounds 4a-d containing Schiff base with morpholine gave compounds 5a-d. All compounds were tested for their antioxidant and antimicrobial activities. The antioxidant test results of DPPH• radical scavenging and ferric reducing/antioxidant power methods showed good antioxidant activity. The triazole-thiol (3) was the most active, and the effect of the substituent type of the thiophene ring on the activity was same for both Schiff bases (4a-d) and Mannich bases (5a-d). Among the newly synthesized triazole derivatives, the Schiff base 4d and the Mannich base 5d carrying nitro substituent on the thiophene ring showed promising antibacterial and antifungal activity, with lower MIC values than the standard antibacterial ampicillin.

  15. Rates of solubilization and biodegradation of PAH compounds in porous media. [Quarterly report

    Energy Technology Data Exchange (ETDEWEB)

    Luthy, R.G.

    1991-11-01

    Microbial degradation of hydrophobic organic compounds in soils and aquifer media is dependent on rates of desorption of these compounds from solids and rates of solubilization from residual nonaqueous phase liquids (NAPLs). The couples processes involving microbial degradation and hydrophobic compound availability are not well understood. The proposed research effort explores certain physicochemical phenomena that may have a significant affect on the rate of microbial degradation of hydrophobic organic compounds in porous media. The investigation will examine rates of biomineralization of polycyclic aromatic hydrocarbon (PAH) compounds that are leached from a residual saturation of coal tar. Batch and continuously-stirred reactor studies will be used to measure solute equilibrium concentrations and rates of solubilization of PAH compounds from coal tar imbided into microporous silica media. These rates will be compared with rates of mineralization of {sup 14}C-labeled compounds in similar systems inoculated with a culture of PAH degrading microorganisms. Column experiments will also be conducted to assess the rates of solubilization and mass transfer coefficients from coal tar entrapped in a sandy aquifer material by capillary forces.

  16. Design, synthesis, crystallization and biological evaluation of new symmetrical biscationic compounds as selective inhibitors of human Choline Kinase α1 (ChoKα1)

    Science.gov (United States)

    Schiaffino-Ortega, Santiago; Baglioni, Eleonora; Mariotto, Elena; Bortolozzi, Roberta; Serrán-Aguilera, Lucía; Ríos-Marco, Pablo; Carrasco-Jimenez, M. Paz; Gallo, Miguel A.; Hurtado-Guerrero, Ramon; Marco, Carmen; Basso, Giuseppe; Viola, Giampietro; Entrena, Antonio; López-Cara, Luisa Carlota

    2016-03-01

    A novel family of compounds derivative of 1,1‧-(((ethane-1,2-diylbis(oxy))bis(4,1-phenylene))bis(methylene))-bispyridinium or -bisquinolinium bromide (10a-l) containing a pair of oxygen atoms in the spacer of the linker between the biscationic moieties, were synthesized and evaluated as inhibitors of choline kinase against a panel of cancer-cell lines. The most promising compounds in this series were 1,1‧-(((ethane-1,2-diylbis(oxy))bis(4,1-phenylene))bis(methylene))bis(4-(dimethylamino)pyridinium) bromide (10a) and 1,1‧-(((ethane-1,2-diylbis(oxy))bis(4,1-phenylene))bis(methylene))-bis(7-chloro-4-(pyrrolidin-1-yl)quinolinium) bromide (10l), which inhibit human choline kinase (ChoKα1) with IC50 of 1.0 and 0.92 μM, respectively, in a range similar to that of the previously reported biscationic compounds MN58b and RSM932A. Our compounds show greater antiproliferative activities than do the reference compounds, with unprecedented values of GI50 in the nanomolar range for several of the cancer-cell lines assayed, and more importantly they present low toxicity in non-tumoral cell lines, suggesting a cancer-cell-selective antiproliferative activity. Docking studies predict that the compounds interact with the choline-binding site in agreement with the binding mode of most previously reported biscationic compounds. Moreover, the crystal structure of ChoKα1 with compound 10a reveals that this compound binds to the choline-binding site and mimics HC-3 binding mode as never before.

  17. Synthesis, Spectroscopy and Antibacterial Activity of Supermolecular Compounds of Organotitanium Substituted Heteropolytungstates Containing 8-Quinolinol%Synthesis, Spectroscopy and Antibacterial Activity of Supermolecular Compounds of Organotitanium Substituted Heteropolytungstates Containing8-Quinolinol

    Institute of Scientific and Technical Information of China (English)

    FENG Chang-gen; XIONG Yu-di; LIU Xia

    2011-01-01

    Parent compounds of cyclopentadienyltitanium substituted heteropolytungstates with Keggin structure, An[(CpTi)XW11O39]· xH2O (A=Me4N, K; X=P, Si, Co; Cp=η5-C5H5) were synthesized in aqueous phase. By allowing parent heteropoly compounds to react with protonated 8-quinolinol, the title supermolecular compounds (C9H8NO)mAn[(CpTi)XW11O39]· xH2O (A=Me4N, H; X=P, Si, Co) were synthesized. The title compounds were characterized by means of elementary analysis, IR, UV, 1 H NMR,XRD and TC-DSC. The results indicate that the title compounds are new heteropoly compounds, and there is a charge transfer interaction between the organic cation and heteropoly anion. The results obtained from thermal analysis show that QCpTiPW, QCpTiSiW and QCpTiCoW begin to decompose at 212.4, 194. 2 and 171.2℃, respectively. The results obtained from antibacterial test reveal that QCpTiSiW has the best antibacterial activity, and the MIC values of QCpTiSiW against Escherichia coli and Staphylococcus aurous are 64. 0 and 0. 500 μg · mL-1 , respectively.

  18. Chemiresistor microsensors for in-situ monitoring of volatile organic compounds : final LDRD report.

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, Michael Loren; Hughes, Robert Clark; Kooser, Ara S.; McGrath, Lucas K.; Ho, Clifford Kuofei; Wright, Jerome L.; Davis, Chad Edward

    2003-09-01

    This report provides a summary of the three-year LDRD (Laboratory Directed Research and Development) project aimed at developing microchemical sensors for continuous, in-situ monitoring of volatile organic compounds. A chemiresistor sensor array was integrated with a unique, waterproof housing that allows the sensors to be operated in a variety of media including air, soil, and water. Numerous tests were performed to evaluate and improve the sensitivity, stability, and discriminatory capabilities of the chemiresistors. Field tests were conducted in California, Nevada, and New Mexico to further test and develop the sensors in actual environments within integrated monitoring systems. The field tests addressed issues regarding data acquisition, telemetry, power requirements, data processing, and other engineering requirements. Significant advances were made in the areas of polymer optimization, packaging, data analysis, discrimination, design, and information dissemination (e.g., real-time web posting of data; see www.sandia.gov/sensor). This project has stimulated significant interest among commercial and academic institutions. A CRADA (Cooperative Research and Development Agreement) was initiated in FY03 to investigate manufacturing methods, and a Work for Others contract was established between Sandia and Edwards Air Force Base for FY02-FY04. Funding was also obtained from DOE as part of their Advanced Monitoring Systems Initiative program from FY01 to FY03, and a DOE EMSP contract was awarded jointly to Sandia and INEEL for FY04-FY06. Contracts were also established for collaborative research with Brigham Young University to further evaluate, understand, and improve the performance of the chemiresistor sensors.

  19. Bridging the Emissions Gap. A UNEP Synthesis Report

    Energy Technology Data Exchange (ETDEWEB)

    Blok, K.; Hoehne, N. [Ecofys, Utrecht (Netherlands); Hare, W. [Potsdam Institute for Climate Research, Potsdam (Germany); Kainuma, M. [National Institute for Environmental Studies NIES, 16-2 Onogawa, Tsukuba-City, Ibaraki, 305-8506 (Japan); Kejun, J. [Energy Research Institute, Beijing (China); Lee, D.S. [Manchester Metropolitan University, Manchester (United Kingdom); Rogelj, J. [ETH Zurich, Zurich (Switzerland); Shukla, P.R. [Indian Institute of Management IIM, AHmedabad (India)

    2011-11-15

    Global climate policy has advanced on several fronts over the past few years and this report deals with two developments of particular importance: The readiness of countries to pledge to new emission reductions, and the agreement among countries to an important global climate target. In December, 2009, countries were encouraged to submit pledges for reducing greenhouse gas emissions for the year 2020 as part of the Copenhagen Accord. Subsequently, 42 industrialized countries and 44 developing countries submitted pledges. At the climate conference in Cancun one year later, parties formally recognised country pledges and decided 'to hold the increase in global average temperature below 2C above pre-industrial levels'. They also left open the option for 'strengthening the long-term global goal on the basis of best available scientific knowledge including in relation to a global average temperature rise of 1.5C'. An obvious and basic question is, to what extent will the country pledges help to meet the 2C and 1.5C targets.

  20. Studies on Synthesis and Biological Activities of Novel Triazole Compounds Containing Pyrimidine or N,N-Dialkyldithiocarbamate Ring

    Institute of Scientific and Technical Information of China (English)

    XU Liang-zhong; ZHANG Shu-sheng; GAO Hong-rong; JIAO Kui

    2003-01-01

    Twelve of the title compounds were synthesized. Their structures were identified by means of IR, EA, 1H NMR and MS. The IR spectra clearly show that the absorptions in the regions of 1716-1666 cm-1 and 1505-1499 cm-1 are the characteristic absorption bands for νC=O and νC=N. In the 1H NMR spectra of target compounds(10a-10g), three protons of a CH-CH2- group present three sets of quartet peaks of the protons. The preliminary bioassays showed that the synthesized compounds exhibited some activities of fungicides and plant growth regulators.

  1. Synthesis and characterization of novel star-shaped pyridine cored compounds with alternating carbazole and triphenylamine moieties

    Institute of Scientific and Technical Information of China (English)

    Ji Bing Yuan; Zhi Guo Zhang; Louis Man Leung; Ke Li Zhang

    2008-01-01

    Amorphous 2,4,6-trissubstituted pyridines containing three peripheral carbazole or two triphenylamine and one carbazole moieties, respectively, have been synthesized and characterized. The properties of the compounds are investigated by UV-visabsorption, photoluminescence spectroscopy, thermal analysis as well as cyclic voltammetry. The results show that the compounds have high thermal stability, emit blue light. Also, the compounds possess the HOMO and LUMO energy levels comparable to those of NPB. The effects of different substituents on the electronic properties of the materials have been discussed.

  2. Facile Synthesis of a Series of Perfluoroalkyl-containing Tetra-spirocyclic Compounds and Their Spectral Analysis

    Institute of Scientific and Technical Information of China (English)

    SHI Zhi-Jian; ZHANG Shun-Li; CAO Wei-Guo; DENG Hong-Mei

    2008-01-01

    An efficient and versatile method was described for the preparation of a series of perfluoroalkyl substituted spiro cyclic compounds 2,17-di(perfluoroalkylmethyl)-3,16-di(iodomethyl)-7,12,20,23-tetraoxatetraspiro-[4.2.2.2.4.2.2.2]tetracosane-6,13,19,24-tetraones,and these perfluoroalkyl-containing tetra-spirocyclic compounds could be useful.At the meantime,all these compounds were fully confirmed by 1H NMR,13C NMR,IR,MS analy-ses and elemental analysis.

  3. Progress on the Synthesis of Indazole Compounds%吲唑类化合物合成研究进展

    Institute of Scientific and Technical Information of China (English)

    曲毅; 张宇; 张辰

    2012-01-01

    This paper reviews some routes of indazole compounds,mainly focuses on the developments of indazole compounds bearing electron donor group (methoxy),synthetic methods and the prospects of indazole compounds.%综述了吲唑类化合物的一些典型合成方法,并重点围绕对含有供电子基团(甲氧基)的吲唑类化合物的研究现状、合成方法以及开发前景等分别进行了阐述。

  4. Synthesis and Odor Evaluation of Five New Sulfur-Containing Ester Flavor Compounds from 4-Ethyloctanoic Acid

    Directory of Open Access Journals (Sweden)

    Baoguo Sun

    2010-07-01

    Full Text Available Five sulfur-containing flavor compounds were synthesized for the first time by the reaction of 4-ethyloctanoyl chloride with sulfur-containing alcohols or mercaptans. The synthesized compounds are 3-(methylthiopropyl 4-ethyloctanoate, 2-methyl-3-tetrahydro-furanthiol 4-ethyloctanoate, 4-methyl-5-thiazoleethanol 4-ethyloctanoate, 2-furan-methanethiol 4-ethyloctanoate and 2-methyl-3-furanthiol 4-ethyloctanoate. These five synthetic sulfur-containing ester flavor compounds all have meaty odor and might be used in foods if approved for this purpose in the future.

  5. Compound odontoma associated with mandibular impacted permanent central incisor: a case report

    Directory of Open Access Journals (Sweden)

    Ugur Gurer

    2012-04-01

    Full Text Available

    Odontomas are the most common benign odontogenic tumors that are hamartomas composed of various dental tissues, and there are two types, complex and compound. Compound odontomas are more prevalent than complex odontomas and consist of many teeth–like structures. Most of such lesions are asymptomatic. These lesions are generally diagnosed by routine radiological examination. The compound type is generally found in the anterior region of the maxilla. The etiology of these lesions has not been precisely explained. If there is absence of any contraindication, the treatment for odontomas is surgical excision.

    This article describes a case of compound odontoma associated with impacted central mandibular right permanent incisor in a 12–year–old female due to trauma. The odontoma was surgically removed with an impacted central incisor.

  6. Alternate fuels and chemicals from synthesis gas: Vinyl acetate monomer. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Richard D. Colberg; Nick A. Collins; Edwin F. Holcombe; Gerald C. Tustin; Joseph R. Zoeller

    1999-01-01

    There has been a long-standing desire on the part of industry and the U.S. Department of Energy to replace the existing ethylene-based vinyl acetate monomer (VAM) process with an entirely synthesis gas-based process. Although there are a large number of process options for the conversion of synthesis gas to VAM, Eastman Chemical Company undertook an analytical approach, based on known chemical and economic principles, to reduce the potential candidate processes to a select group of eight processes. The critical technologies that would be required for these routes were: (1) the esterification of acetaldehyde (AcH) with ketene to generate VAM, (2) the hydrogenation of ketene to acetaldehyde, (3) the hydrogenation of acetic acid to acetaldehyde, and (4) the reductive carbonylation of methanol to acetaldehyde. This report describes the selection process for the candidate processes, the successful development of the key technologies, and the economic assessments for the preferred routes. In addition, improvements in the conversion of acetic anhydride and acetaldehyde to VAM are discussed. The conclusion from this study is that, with the technology developed in this study, VAM may be produced from synthesis gas, but the cost of production is about 15% higher than the conventional oxidative acetoxylation of ethylene, primarily due to higher capital associated with the synthesis gas-based processes.

  7. Synthesis and characterization of a novel rhodamine labeled cholesterol reporter.

    Science.gov (United States)

    Maiwald, Alexander; Bauer, Olivia; Gimpl, Gerald

    2017-06-01

    We introduce the novel fluorescent cholesterol probe RChol in which a sulforhodamine group is linked to the sixth carbon atom of the steroid backbone of cholesterol. The same position has recently been selected to generate the fluorescent reporter 6-dansyl-cholestanol (DChol) and the photoreactive 6-azi-cholestanol. In comparison with DChol, RChol is brighter, much more photostable, and requires less energy for excitation, i.e. favorable conditions for microscopical imaging. RChol easily incorporates into methyl-β-cyclodextrin forming a water-soluble inclusion complex that acts as an efficient sterol donor for cells and membranes. Like cholesterol, RChol possesses a free 3'OH group, a prerequisite to undergo intracellular esterification. RChol was also able to support the growth of cholesterol auxotrophic cells and can therefore substitute for cholesterol as a major component of the plasma membrane. According to subcellular fractionation, slight amounts of RChol (~12%) were determined in low-density Triton-insoluble fractions whereas the majority of RChol was localized in non-rafts fractions. In phase-separated giant unilamellar vesicles, RChol preferentially partitions in liquid-disordered membrane domains. Intracellular RChol was transferred to extracellular sterol acceptors such as high density lipoproteins in a dose-dependent manner. Unlike DChol, RChol was not delivered to the cholesterol storage pathway. Instead, it translocated to endosomes/lysosomes with some transient contacts to peroxisomes. Thus, RChol is considered as a useful probe to study the endosomal/lysosomal pathway of cholesterol. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. The nature of the potassium compound acting as a promoter in iron-alumina catalysts for ammonia synthesis

    NARCIS (Netherlands)

    Ommen, van J.G.; Bolink, W.J.; Prasad, J.; Mars, P.

    1975-01-01

    The chemical form of the potassium promoter on an iron-alumina catalyst during ammonia synthesis has been studied by two methods, viz, (i) the measurement of the equilibrium constant of the process KNH2 + H2 KH + NH3, and (ii) chemical analysis of the used catalyst. The equilibrium constant measurem

  9. Synthesis of a Photoluminescent and Triboluminescent Copper(I) Compound: An Experiment for an Advanced Inorganic Chemistry Laboratory

    Science.gov (United States)

    Marchetti, Fabio; Di Nicola, Corrado; Pettinari, Riccardo; Timokhin, Ivan; Pettinari, Claudio

    2012-01-01

    A simple synthesis is proposed from inexpensive reactants of a copper(I) derivative that exhibits strong photoluminescence and, in the crystalline form, exhibits strong triboluminescence. This laboratory provides an opportunity for introducing students to the phenomenon of triboluminescence. (Contains 1 scheme and 4 figures.)

  10. Synthesis of azomethine macrocycles by condensation of dicarbonyl compounds with diamines without using metal ions as template agents

    Energy Technology Data Exchange (ETDEWEB)

    Borisova, Natalia E; Reshetova, Marina D; Ustynyuk, Yuri A [Department of Chemistry, M.V. Lomonosov Moscow State University, Moscow (Russian Federation)

    2007-09-30

    Different strategies for the synthesis of symmetrical and unsymmetrical macrocyclic Schiff bases in the absence of metal ions are considered. General methods for performing macrocyclisation under thermodynamic or kinetic control are analysed. The key factors influencing the structure of macrocyclic azomethines are discussed.

  11. Studies in group IV organometallic chemistry XXX. Synthesis of compounds containing tin---titanium and tin---zirconium bonds

    NARCIS (Netherlands)

    Creemers, H.M.J.C.; Verbeek, F.; Noltes, J.G.

    1968-01-01

    Starting from the tetrakis(diethylamino) derivatives of titanium and zirconium and pheyltin hydrides six intermetalic compounds contianing up to nine tin and titanium(or zirconium) atoms have been obtained by hydrostannolysis type reactions.

  12. Design and synthesis of a heterocyclic compound collection for probing the spatial charactistics of ATP binding sites

    CSIR Research Space (South Africa)

    Kenyon, CP

    2006-02-28

    Full Text Available -specific inhibitors which interact with only a limited group of kinases. The preparation of a collection of small heterocyclic compounds to probe differences in the spatial characteristics of ATP binding sites across the kinome is described...

  13. Studies in group IV organometallic chemistry XXX. Synthesis of compounds containing tin---titanium and tin---zirconium bonds

    NARCIS (Netherlands)

    Creemers, H.M.J.C.; Verbeek, F.; Noltes, J.G.

    Starting from the tetrakis(diethylamino) derivatives of titanium and zirconium and pheyltin hydrides six intermetalic compounds contianing up to nine tin and titanium(or zirconium) atoms have been obtained by hydrostannolysis type reactions.

  14. Yttrium (III chloride catalyzed Mannich reaction: An efficient procedure for the synthesis of β-amino carbonyl compounds

    Directory of Open Access Journals (Sweden)

    Venkateswarlu Yekkirala

    2014-12-01

    Full Text Available Yttrium (III chloride catalyzed Mannich reaction of aldehydes with ketones and amines in acetonitrile at reflux temperature to give various β-amino carbonyl compounds in very good yields.

  15. Design, synthesis, and antihypertensive activity of curcumin-inspired compounds via ACE inhibition and vasodilation, along with a bioavailability study for possible benefit in cardiovascular diseases

    Directory of Open Access Journals (Sweden)

    Zhuang XD

    2016-01-01

    Full Text Available Xiao-dong Zhuang,1,* Li-zhen Liao,2,* Xiao-bian Dong,1 Xun Hu,1 Yue Guo,1 Zhi-min Du,1 Xin-xue Liao,1 Li-chun Wang1 1Department of Cardiology, First Affiliated Hospital, Sun Yat-sen University, Guangzhou, People’s Republic of China; 2Department of Health, Guangdong Pharmaceutical University, Guangzhou Higher Education Mega Center, Guangzhou, People’s Republic of China *These authors contributed equally to this work Abstract: This study describes the synthesis of a novel series of curcumin-inspired compounds via a facile synthetic route. The structures of these derivatives were ascertained using various spectroscopic and analytic techniques. The pharmacological effects of the target analogs were assessed by assaying their inhibition of angiotensin-converting enzyme (ACE. All of the synthesized derivatives exhibited considerable inhibition of ACE, with half-maximal inhibitory concentrations ranging from 1.23 to 120.32 µM. In a docking analysis with testicular ACE (tACE, the most promising inhibitor (4j was efficiently accommodated in the deep cleft of the protein cavity, making close interatomic contacts with Glu162, His353, and Ala356, comparable with lisinopril. Compounds 4i, 4j, 4k, and 4l were further selected for determination of their vasodilator activity (cardiac output and stroke volume on isolated rat hearts using the Langendorff technique. The bioavailability of compound 4j was determined in experimental mice. Keywords: curcumin, synthesis, ACE inhibition, antihypertensive, vasodilation, bioavail­ability

  16. Palladium-Catalyzed Tandem Carbene Migratory Insertion and Intramolecular Cyclization: Synthesis of Chromeno[4,3-b]chromene Compounds.

    Science.gov (United States)

    Shang, Xue Song; Li, Nian Tai; Siyang, Hai Xiao; Liu, Pei Nian

    2015-05-01

    Chromeno[4,3-b]chromene is a ubiquitous structural motif found in various pharmaceuticals and biologically active compounds. A concise palladium-catalyzed reaction of vinyl iodides and salicyl N-tosylhydrazones has been achieved to afford a series of compounds containing the chromeno[4,3-b]chromene scaffold in moderate to high yield. This tandem reaction involves palladium(II) carbene migratory insertion and intramolecular cyclization assisted by an O nucleophile and tolerates various functional groups.

  17. Highly efficient synthesis of quinoxaline derivatives from 1,2-benzenediamine and α-aminoxylated 1,3-dicarbonyl compounds.

    Science.gov (United States)

    Yan, Jianwei; Xu, Yanhong; Zhuang, Fangfang; Tian, Jie; Zhang, Guisheng

    2016-05-01

    Simple and efficient synthetic procedures for the preparation of quinoxaline, pyrazine, pyridopyrazine, and benzoxazin-2-one derivatives were developed. The one-pot cascade process involves the acidic elimination of α-aminoxylated dicarbonyl compounds to generate 1,2,3-tricarbonyl compounds and subsequent condensation with 1,4-N,N or -N,O dinucleophiles to afford quinoxaline, pyrazine, pyridopyrazine, and benzoxazin-2-one scaffolds. All the proposed processes do not need extra catalysts, dry solvents, or harsh reaction conditions.

  18. Potential bioactive Schiff base compounds: Synthesis, characterization, X-ray structures, biological screenings and interaction with Salmon sperm DNA

    Science.gov (United States)

    Sirajuddin, Muhammad; Uddin, Noor; Ali, Saqib; Tahir, Muhammad Nawaz

    2013-12-01

    Three Schiff base compounds ofN‧-substituted benzohydrazide and sulfonohydrazide derivatives: N‧-(2-hydroxy-3-methoxybenzylidene)-4-tert-butyl- benzohydrazide (1), N‧-(5-bromo-2-hydroxybenzylidene)-4-tert-butylbenzohydrazide (2) and N‧-(2-hydroxy-3-methoxybenzylidene)-4-methylbenzenesulfonohydrazide (3) were synthesized and characterized by elemental analysis, FT-IR, 1H, 13C NMR spectroscopy and single crystal analysis. The title compounds have been screened for their biological activities including, antibacterial, antifungal, antioxidant, cytotoxic, enzymatic activities as well as interaction with SS-DNA which showed remarkable activities in each area of research. The DNA binding of the compounds 1-3 with SS-DNA has been carried out with absorption spectroscopy, which reveals the binding propensity towards SS-DNA via intercalation mode of interaction. The intercalative mode of interaction is also supported by viscometric results. The synthesized compounds were also found to be effective against alkaline phosphatase enzyme. They also show significant to good antimicrobial activity against six bacterial and five fungal strains. The MIC (minimum inhibitory concentration) for antibacterial activity ranges from 1.95-500 μg/mL. Compounds 1-3 show cytotoxic activity comparable to the control. At higher conc. (100 μg/L) compound 3 shows 100% activity means that it has killed all brine shrimps. They were also found to be effective antioxidant of 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) and show almost comparable antioxidant activity to that of the standard and known antioxidant, ascorbic acid.

  19. Synthesis and antibacterial evaluation of a novel series of synthetic phenylthiazole compounds against methicillin-resistant Staphylococcus aureus (MRSA).

    Science.gov (United States)

    Mohammad, Haroon; Reddy, P V Narasimha; Monteleone, Dennis; Mayhoub, Abdelrahman S; Cushman, Mark; Seleem, Mohamed N

    2015-04-13

    Methicillin-resistant Staphylococcus aureus infections are a significant global health challenge in part due to the emergence of strains exhibiting resistance to nearly all classes of antibiotics. This underscores the urgent need for the rapid development of novel antimicrobials to circumvent this burgeoning problem. Previously, whole-cell screening of a library of 2,5-disubstituted thiazole compounds revealed a lead compound exhibiting potent antimicrobial activity against MRSA. The present study, conducting a more rigorous analysis of the structure-activity relationship of this compound, reveals a nonpolar, hydrophobic functional group is favored at thiazole-C2 and an ethylidenehydrazine-1-carboximidamide moiety is necessary at C5 for the compound to possess activity against MRSA. Furthermore, the MTS assay confirmed analogs 5, 22d, and 25 exhibited an improved toxicity profile (not toxic up to 40 μg/mL to mammalian cells) over the lead 1. Analysis with human liver microsomes revealed compound 5 was more metabolically stable compared to the lead compound (greater than eight-fold improvement in the half-life in human liver microsomes). Collectively the results presented demonstrate the novel thiazole derivatives synthesized warrant further exploration for potential use as future antimicrobial agents for the treatment of multidrug-resistant S. aureus infections.

  20. Novel multicomponent synthesis of 2,9-dihydro-9-methyl-2-oxo-4-aryl- 1-pyrido[2,3-]indole-3-carbonitrile compounds

    Indian Academy of Sciences (India)

    Saman Damavandi; Reza Sandaroos

    2013-01-01

    Novel multicomponent approach for the synthesis of 2,9-dihydro-2-oxo-4-aryl-1-pyrido[2,3-]indole-3-carbonitrile derivatives via one-pot cyclocondensation reaction of substituted (triethoxymethyl) arene, 1-methyl-1-indol-2-ol and cyanoacetamide in the presence of silica supported ionic liquid [pmim]HSO4SiO2 (silica-supported 1-methyl-3-(triethoxysilylpropyl)imidazolium hydrogensulphate) has been reported.

  1. Synthesis and Characterization of Organotin(IV N-Benzyl-N-Isopropyldithiocarbamate Compounds: Cytotoxic Assay on Human Hepatocarcinoma Cells (HepG2

    Directory of Open Access Journals (Sweden)

    Normah Awang

    2010-01-01

    Full Text Available Problem statement: Several studies on organotin(IV dithiocarbamate compounds have been carried out but not on the synthesis and characterization together with cytotoxic assay of organotin(IV N-benzyl-N-isopropyldithiocarbamate compounds. Approach: Three new organotin(IV compounds of type N-benzyl-N-isopropyldithiocarbamate have been successfully synthesized by direct reaction between secondary amine with organotin(IV chloride using in situ method. All the compounds were characterized using elemental analysis, gravimetric analysis, infrared spectroscopy and Nuclear Magnetic Resonance (NMR spectroscopy. Results: Elemental and gravimetric analyses data of these compounds showed that agreed with the predicted formula, (CH32Sn[S2CN(C7H7(i-C3H7]2 (1, (C4H72Sn[S2CN(C7H7(i-C3H7]2 (2 and (C6H53Sn[S2CN(C7H7(i-C3H7] (3. The infrared spectra of these compounds showed the thioureide bond, v(C=N which occurred at 1438-1440 cm-1 and the v(C=S band appeared in the range of 967-973 cm-1. The presence of the v(C=N and v(C=S bands in the infrared spectra confirmed the presence of dithiocarbamate ligand in that compounds. The bond between sulphur and tin atom were supported with the presence of peak in the range of 365-445 cm-1 that known to be as stretching mode of v(Sn-S. The most important signal in the 13C NMR spectra was the chemical shift of NCS2 group. The 13C NMR spectra of these compound showed a chemical shift in 195.06-202.65 ppm range, which is attributed to the carbon atom of NCS2 group. The crystal structure of compound 2 (dibutyltin(IV N-benzyl-N-isopropyldithiocarbamate has been determined by X-ray single crystal analysis, which shows unsymmetrical nature of the ligand towards coordination to tin. It crystallizes in triclinic P1 space group with the crystal cell parameter: a = 17.7745 (2 (�, b = 19.5463 (3 (�, c = 26.2062 (4 (�, α = 102.5254 (7�, β = 95.1492 (7�, γ= 110.2569 (8�, Z = 10, V (�3 = 8202.1 (2

  2. Convergent and sequential synthesis designs: implications for conducting and reporting systematic reviews of qualitative and quantitative evidence.

    Science.gov (United States)

    Hong, Quan Nha; Pluye, Pierre; Bujold, Mathieu; Wassef, Maggy

    2017-03-23

    Systematic reviews of qualitative and quantitative evidence can provide a rich understanding of complex phenomena. This type of review is increasingly popular, has been used to provide a landscape of existing knowledge, and addresses the types of questions not usually covered in reviews relying solely on either quantitative or qualitative evidence. Although several typologies of synthesis designs have been developed, none have been tested on a large sample of reviews. The aim of this review of reviews was to identify and develop a typology of synthesis designs and methods that have been used and to propose strategies for synthesizing qualitative and quantitative evidence. A review of systematic reviews combining qualitative and quantitative evidence was performed. Six databases were searched from inception to December 2014. Reviews were included if they were systematic reviews combining qualitative and quantitative evidence. The included reviews were analyzed according to three concepts of synthesis processes: (a) synthesis methods, (b) sequence of data synthesis, and (c) integration of data and synthesis results. A total of 459 reviews were included. The analysis of this literature highlighted a lack of transparency in reporting how evidence was synthesized and a lack of consistency in the terminology used. Two main types of synthesis designs were identified: convergent and sequential synthesis designs. Within the convergent synthesis design, three subtypes were found: (a) data-based convergent synthesis design, where qualitative and quantitative evidence is analyzed together using the same synthesis method, (b) results-based convergent synthesis design, where qualitative and quantitative evidence is analyzed separately using different synthesis methods and results of both syntheses are integrated during a final synthesis, and (c) parallel-results convergent synthesis design consisting of independent syntheses of qualitative and quantitative evidence and an

  3. Facile synthesis of poly(ionic liquid)-bonded magnetic nanospheres as a high-performance sorbent for the pretreatment and determination of phenolic compounds in water samples.

    Science.gov (United States)

    Bi, Wentao; Wang, Man; Yang, Xiaodi; Row, Kyung Ho

    2014-07-01

    Poly(ionic liquid)-bonded magnetic nanospheres were easily synthesized and applied to the pretreatment and determination of phenolic compounds in water samples, which have detrimental effects on water quality and the health of living beings. The high affinity of poly(ionic liquid)s toward the target compounds as well as the magnetic behavior of Fe3 O4 were combined in this material to provide an efficient and simple magnetic solid-phase extraction approach. The adsorption behavior of the poly(ionic liquid)-bonded magnetic nanospheres was examined to optimize the synthesis. Different parameters affecting the magnetic solid-phase extraction of phenolic compounds were assessed in terms of adsorption and recovery. Under the optimal conditions, the proposed method showed excellent detection sensitivity with limits of detection in the range of 0.3-0.8 ng/mL and precision in the range of 1.2-3.3%. This method was also applied successfully to the analysis of real water samples; good spiked recoveries over the range of 82.5-99.2% were obtained. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Synthesis,Characterization and Thermodynamic Study of the Solid State Coordination Compound Ni(Nic)2·H2O(s)(Nic=Nicotinate)

    Institute of Scientific and Technical Information of China (English)

    CHEN Jingtao; HE Donghua; DI Youying; KONG Yuxia; YANG Weiwei; DAN Wenyan; TAN Zhicheng

    2009-01-01

    A novel compound-monohydrated nickel nicotinate was synthesized by the method of room temperature solid phase synthesis and ball grinder.FT1R,chemical and elemental analysis,TG/DTG,and X-ray powder diffraction technique were applied to characterize the structure and composition of the coordination compound.Low-temperature heat capacities of the solid coordination compound have been measured by a precision automated adiabatic calorimeter over the temperature range from 78 to 386 K.A solid-solid phase transition occurred in the temperature range of 328-358 K in the heat capacity curve,and the peak temperature,the molar enthalpy and moties in the temperature ranges of 78-328 K and 358-386 K were fitted to two polynomials,respectively.The polynomial fitted values of the molar heat capacities and fundamental thermodynamic functions of the sample relative to the standard reference temperature 298.15 K were calculated and tabulated at the intervals of 5 K.

  5. Using docking and alchemical free energy approach to determine the binding mechanism of eEF2K inhibitors and prioritizing the compound synthesis.

    Science.gov (United States)

    Wang, Qiantao; Edupuganti, Ramakrishna; Tavares, Clint D J; Dalby, Kevin N; Ren, Pengyu

    2015-01-01

    A-484954 is a known eEF2K inhibitor with submicromolar IC50 potency. However, the binding mechanism and the crystal structure of the kinase remains unknown. Here, we employ a homology eEF2K model, docking and alchemical free energy simulations to probe the binding mechanism of eEF2K, and in turn, guide the optimization of potential lead compounds. The inhibitor was docked into the ATP-binding site of a homology model first. Three different binding poses, hypothesis 1, 2, and 3, were obtained and subsequently applied to molecular dynamics (MD) based alchemical free energy simulations. The calculated relative binding free energy of the analogs of A-484954 using the binding pose of hypothesis 1 show a good correlation with the experimental IC50 values, yielding an r (2) coefficient of 0.96 after removing an outlier (compound 5). Calculations using another two poses show little correlation with experimental data, (r (2) of less than 0.5 with or without removing any outliers). Based on hypothesis 1, the calculated relative free energy suggests that bigger cyclic groups, at R1 e.g., cyclobutyl and cyclopentyl promote more favorable binding than smaller groups, such as cyclopropyl and hydrogen. Moreover, this study also demonstrates the ability of the alchemical free energy approach in combination with docking and homology modeling to prioritize compound synthesis. This can be an effective means of facilitating structure-based drug design when crystal structures are not available.

  6. Two new CuI compounds with zwitterionic tetrazolate ligand: In situ synthesis, crystal structures, luminescence and photocatalytic properties

    Science.gov (United States)

    Zhang, Jian-Yong; Xing, Yuan-Yuan; Wang, Qing-Wei; Zhang, Na; Deng, Wei; Gao, En-Qing

    2015-12-01

    Two 2D new Cu(I) coordination polymers, namely [Cu2(mpTZ)2Br2]·H2O (1), and [Cu2(mpTZ)2N3]ClO4 (2) (mpTZ=N-methyl-4-pyridinium tetrazolate) have been synthesized under solvothermal conditions, in which the mpTZ ligands and CuI ions were obtained through in situ [2+3] cycloaddition reaction and reduction reaction of CuII salts, respectively. Both compounds have been structural characterized by single crystal X-ray diffraction, FT-IR, PXRD and EA. Compound 1 exhibits a 2D neutral coordination network, in which the CuI ions are bridged by η3-1, 2, 4-tetrazolate into 2D sheet. In compound 2, the CuI ions are linked by azide (in μ3-1, 1, 3 bridging mode) and tetrazolate (in η3-1, 2, 3 bridging mode) anions into 2D positively charged sheet, extended along the bc plane. Both compounds 1 and 2 exhibit intense bluish green luminescence in the solid state. Photocatalytic performances of the two compounds for the degradation of methylene blue (MB) under visible light were also investigated and the MB degradation in the presence of 1 was nearly complete (99%) after 150 min.

  7. Design and synthesis of potent N-acylethanolamine-hydrolyzing acid amidase (NAAA inhibitor as anti-inflammatory compounds.

    Directory of Open Access Journals (Sweden)

    Yuhang Li

    Full Text Available N-acylethanolamine-hydrolyzing acid amidase (NAAA is a lysosomal enzyme involved in biological deactivation of N-palmitoylethanolamide (PEA, which exerts anti-inflammatory and analgesic effects through the activation of nuclear receptor peroxisome proliferator-activated receptor-alpha (PPAR-α. To develop selective and potent NAAA inhibitors, we designed and synthesized a series of derivatives of 1-pentadecanyl-carbonyl pyrrolidine (compound 1, a general amidase inhibitor. Structure activity relationship (SAR studies have identified a compound 16, 1-(2-Biphenyl-4-ylethyl-carbonyl pyrrolidine, which has shown the highest inhibition on NAAA activity (IC(50 =2.12 ± 0.41 µM and is characterized as a reversible and competitive NAAA inhibitor. Computational docking analysis and mutagenesis study revealed that compound 16 interacted with Asparagine 209 (Asn(209 residue flanking the catalytic pocket of NAAA so as to block the substrate entrance. In vitro pharmacological studies demonstrated that compound 16 dose-dependently reduced mRNA expression levels of iNOS and IL-6, along with an increase of intracellular PEA levels, in mouse macrophages with lipopolysaccharides (LPS induced inflammation. Our study discovered a novel NAAA inhibitor, compound 16, that could serve as a potential anti-inflammatory agent.

  8. Synthesis and bioactive evaluations of novel benzotriazole compounds as potential antimicrobial agents and the interaction with calf thymus DNA

    Indian Academy of Sciences (India)

    Yu Ren; Hui Zhen Zhang; Shao Lin Zhang; Yun Lei Luo; Ling Zhang; Cheng He Zhou; Rong Xia Geng

    2015-12-01

    A novel series of benzotriazole derivatives were synthesized and characterized by NMR, IR and MS spectra. The bioactive assay manifested that most of the new compounds exhibited moderate to good antibacterial and antifungal activities against the tested strains in comparison to reference drugs chloromycin, norfloxacin and fluconazole. Especially, 2,4-dichlorophenyl substituted benzotriazole derivative 6f displayed good antibacterial activity against MRSA with MIC value of 4 g/mL, which was 2-fold more potent than Chloromycin, and it also displayed 3-fold stronger antifungal activity (MIC = 4 g/mL) than fluconazole (MIC = 16 g/mL) against Beer yeast. The preliminary interactive investigations of compound 6f with calf thymus DNA revealed that compound 6f could effectively intercalate into DNA to form compound 6f–DNA complex which might block DNA replication to exert antimicrobial activities. Molecular docking experiments suggested that compound 6f projected into base-pairs of DNA hexamer duplex forming two hydrogen bonds with guanine of DNA. The theoretical calculations were in accordance with the experimental results.

  9. "Meshed-Bag Gathered-Bunch" method for solid-phase synthesis of small molecular diverse compounds.

    Science.gov (United States)

    Zhang, Suo-De; Liu, Gang; Xia, Shu-Quan; Wu, Ping; Zhang, Liang

    2002-01-01

    A new "Meshed-Bag Gathered-Bunch" technology for the solid-phase synthesis of chemical libraries was developed. Using such technology, we synthesized muramyl dipeptide mimetics including derivatives at the N- and C-terminus, cyclic muramyl dipeptide mimetics, muramyl dipeptide and Tuftsin's analogue conjugates. The advantages of such a method include ease of manufacture, low unit cost of production, the physical encoding method, and the compatibility with both parallel and "split-mix" approaches.

  10. Synthesis and Structural Characterization of New High-Valent Inorganic Fluorine Compounds and their Oxidizing Properties. Volume 2

    Science.gov (United States)

    1992-02-01

    Schrobilgen, and Richard F. W. Bader* Received August 17, 1988 The recent synthesis of a salt of FKr-NCH 5, together with the earlier preparation of its Xe...oif thc scissoring deformavtion muode for tlie scric’. (321 (,hie, rV F0 *. WilsoriItgn 1j 1 ilnwS hn 1975 , 14. M 2#4 (3.hisý SharF , C aIndv C hro

  11. Ionic-liquid-supported (ILS) catalysts for asymmetric organic synthesis.

    Science.gov (United States)

    Ni, Bukuo; Headley, Allan D

    2010-04-19

    The asymmetric synthesis of compounds that contain new C-C and C-O bonds remains one of the most important types of synthesis in organic chemistry. Over the years, many different types of catalysts have been designed and used effectively to carry out such transformations. Ionic-liquid-supported (ILS) catalysts represent a new and very effective class of catalysts that are used to facilitate the asymmetric synthesis of such compounds. There are many advantages to using ILS catalysts; they are nontoxic, environmentally benign, and, most important, recyclable. An overview of the design, synthesis, mode of action, and effectiveness of this class of catalysts is reported.

  12. Synthesis Report

    DEFF Research Database (Denmark)

    Attila, Károly; Gács, János; Hunya, Gabor

    From the beginning of transition in 1989/90, the CEECs switched towards an ‘open economy’ model of economic development, and the evolving patterns of trade, industrial specialization and integration into cross-border production networks through foreign direct investment (FDI) have played a crucia...... an appropriate policy mix to foster competitiveness via trade and FDI. Against this backdrop, research in this work package provides an update of the role and further potential of internationalization processes for the region’s economic cohesion and growth.......From the beginning of transition in 1989/90, the CEECs switched towards an ‘open economy’ model of economic development, and the evolving patterns of trade, industrial specialization and integration into cross-border production networks through foreign direct investment (FDI) have played a crucial...... role in structural changes and modernisation processes of CEECs’ economies. 2 However, the economic crisis and the rise of global competition from other, mainly Asian, emerging economies challenge the future sustainability of the development model adopted by CEECs. This triggers also questions about...

  13. Synthesis Report

    DEFF Research Database (Denmark)

    Attila, Károly; Gács, János; Hunya, Gabor;

    From the beginning of transition in 1989/90, the CEECs switched towards an ‘open economy’ model of economic development, and the evolving patterns of trade, industrial specialization and integration into cross-border production networks through foreign direct investment (FDI) have played a crucial...

  14. Synthesis and Biological Investigation of Δ(12)-Prostaglandin J3 (Δ(12)-PGJ3) Analogues and Related Compounds.

    Science.gov (United States)

    Nicolaou, K C; Pulukuri, Kiran Kumar; Rigol, Stephan; Heretsch, Philipp; Yu, Ruocheng; Grove, Charles I; Hale, Christopher R H; ElMarrouni, Abdelatif; Fetz, Verena; Brönstrup, Mark; Aujay, Monette; Sandoval, Joseph; Gavrilyuk, Julia

    2016-05-25

    A series of Δ(12)-prostaglandin J3 (Δ(12)-PGJ3) analogues and derivatives were synthesized employing an array of synthetic strategies developed specifically to render them readily available for biological investigations. The synthesized compounds were evaluated for their cytotoxicity against a number of cancer cell lines, revealing nanomolar potencies for a number of them against certain cancer cell lines. Four analogues (2, 11, 21, and 27) demonstrated inhibition of nuclear export through a covalent addition at Cys528 of the export receptor Crm1. One of these compounds (i.e., 11) is currently under evaluation as a potential drug candidate for the treatment of certain types of cancer. These studies culminated in useful and path-pointing structure-activity relationships (SARs) that provide guidance for further improvements in the biological/pharmacological profiles of compounds within this class.

  15. 含二茂铁基Shiff碱的合成%Synthesis of the compound containing ferrocenyl Schiff base

    Institute of Scientific and Technical Information of China (English)

    张鑫; 侯雪梅; 闫丽; 李传碧

    2009-01-01

    本文由呋喃甲酸经酯化、酰肼化反应得到呋喃甲酸酰肼,再由乙酰二茂铁与呋喃甲酸酰肼在乙醇溶剂中反应得到含二茂铁基的呋喃甲酸酰腙,以红外光谱、核磁共振谱对产品进行确定.%In this paper, we used (a-)furancarboxylic acid as raw material, the compound of furan-2-caraoxylic acid hydrazide was synthesized by the ester spending reaction. The acyl hydrazine spending reaction;acetylferrocene reacted with furan-2-caraoxylic acid hydrazide in ethanol to give the compound containing ferrocenyl Schiff base furan-2-caraoxylic acid acyi hydrazone, the compound was determined by IR and 1HNMR spectrometer.

  16. Synthesis and Magnetic Properties of the Intercalation Compound FePS3 (CoCp2)0.40

    Institute of Scientific and Technical Information of China (English)

    LIN Jun; DAI Yao-Dong; HE Yun; HUANG Hong-Bo; XIAO Fan; XIA Yuan-Fu

    2004-01-01

    @@ Intercalation compound FePS3 (CoCp2 )0.40 (CoCp2 = cobaltocene) was synthesized, and the crystal structure and magnetic properties were studied by x-ray diffraction, magnetic susceptibility measurement, and Mossbauer spectroscopy. The crystal structure was indexed to monoclinic unit cell with a = 5.996A, b = 10.106A, c =12.511 A, β = 105.916°, and about 5.6 A expansion at the c-direction compared to pure FePS3. The Mossbauer spectra indicate that there are three kinds of divalent ions with high spin state in the intercalation compound,which implies charge transfer from guest to the Fe-S e*g anti-bonding orbits of the host lattice. No cationic vacancies are formed in the intercalation compound. The ferromagnetism at low temperature originates from the spin canting of divalent ions.

  17. Synthesis of Four Triazole Compounds and Their Corrosion Inhibitive Effect on Carbon Steel in Hydrochloric Acid Medium

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xiao-Ru; XU Min-Hua; ZHANG Shu-Sheng

    2008-01-01

    Four new 1,2,3-triazoles (3a, 3b, 4a and 4b) have been synthesized selectively via click chemistry approach and characterized by elemental analysis, IR, 1H NMR, 13C NMR and single crystal X-ray crystallographic analysis. The inhibiting action of these compounds against the corrosion of carbon steel in 1.0 mol/L HCI solution was investigated by electrochemical techniques including polarization and electrochemical impedance spectroscopy (EIS), both results of which indicate that these compounds act as good anodic inhibitors. The electrochemical study also shows that 4b is the best inhibitor among the four compounds in this work and its efficiency increases with concentration.The obtained highest IE (inhibition efficiency) of 4b is around 97%.

  18. Novel platinum(II) compounds with O,S bidentate ligands: synthesis, characterization, antiproliferative properties and biomolecular interactions.

    Science.gov (United States)

    Mügge, Carolin; Liu, Ruiqi; Görls, Helmar; Gabbiani, Chiara; Michelucci, Elena; Rüdiger, Nadine; Clement, Joachim H; Messori, Luigi; Weigand, Wolfgang

    2014-02-28

    Cisplatin and its analogues are first-line chemotherapeutic agents for the treatment of numerous human cancers. A major inconvenience in their clinical use is their strong tendency to link to sulfur compounds, especially in kidney, ultimately leading to severe nephrotoxicity. To overcome this drawback we prepared a variety of platinum complexes with sulfur ligands and analyzed their biological profiles. Here, a series of six platinum(II) compounds bearing a conserved O,S binding moiety have been synthesized and characterized as experimental anticancer agents. The six compounds differ in the nature of the O,S bidentate β-hydroxydithiocinnamic alkyl ester ligand where both the substituents on the aromatic ring and the length of the alkyl chain may be varied. The two remaining coordination positions at the square-planar platinum(II) center are occupied by a chloride ion and a DMSO molecule. These novel platinum compounds showed an acceptable solubility profile in mixed DMSO-buffer solutions and an appreciable stability at physiological pH as judged from analysis of their time-course UV-visible absorption spectra. Their anti-proliferative and pro-apoptotic activities were tested against the cisplatin-resistant lung cancer cell line A549. Assays revealed significant effects of the sample drugs at low concentrations (in the μmolar range); initial structure-activity-relationships are proposed. The activity of the apoptosis-promoting protein caspase 3/7 was determined; results proved that these novel platinum compounds, under the chosen experimental conditions, preferentially induce apoptosis over necrosis. Reactions with the model proteins cytochrome c, lysozyme and albumin were studied by ESI MS and ICP-OES to gain preliminary mechanistic information. The tested compounds turned out to metalate the mentioned proteins to a large extent. In view of the obtained results these novel platinum complexes qualify themselves as promising cytotoxic agents and merit, in our

  19. Synthesis and structure of bis(-dibenzoyl methanato -O,O′) (aquo-O) dioxouranium (VI) compound

    Indian Academy of Sciences (India)

    S Kannan; M G B Drew

    2014-09-01

    The compound [UO2(C6H5COCHCOC6H5)2.H2O] was synthesized and characterized by IR, 1H NMR and CHN analysis. Structure of the compound shows that the uranium atom is surrounded by seven oxygen atoms in a pentagonal bi-pyramidal geometry. The water molecule is hydrogen bonded to another molecule via the uranyl and -diketonate oxygen atoms to give a linear zig-zag arrangement along the `a' axis. The whole molecule is stabilized in solid state by various intermolecular hydrogen bonding interactions.

  20. Synthesis of indazoles by the [3+2] cycloaddition of diazo compounds with arynes and subsequent acyl migration.

    Science.gov (United States)

    Liu, Zhijian; Shi, Feng; Martinez, Pablo D G; Raminelli, Cristiano; Larock, Richard C

    2008-01-04

    The [3+2] cycloaddition of a variety of diazo compounds with o-(trimethylsilyl)aryl triflates in the presence of CsF or TBAF at room temperature provides a very direct, efficient approach to a wide range of potentially biologically and pharmaceutically interesting substituted indazoles in good to excellent yields under mild reaction conditions. Simple diazomethane derivatives afford N-unsubstituted indazoles or 1-arylated indazoles, depending upon the stoichiometry of the reagents and the reaction conditions, while dicarbonyl-containing diazo compounds undergo carbonyl migration to afford 1-acyl or 1-alkoxycarbonyl indazoles selectively.

  1. Two half-sandwiched ruthenium (II compounds containing 5-fluorouracil derivatives: synthesis and study of DNA intercalation.

    Directory of Open Access Journals (Sweden)

    Zhao-Jun Li

    Full Text Available Two novel coordination compounds of half-sandwiched ruthenium(II containing 2-(5-fluorouracil-yl-N-(pyridyl-acetamide were synthesized, and their intercalation binding modes with calf thymus DNA were revealed by hyperchromism of ultraviolet-visible spectroscopy; the binding constants were determined according to a Langmuir adsorption equation that was deduced on the base of careful cyclic voltammetry measurements. The two compounds exhibited DNA intercalation binding activities with the binding constants of 1.13×106 M-1 and 5.35 ×105 M-1, respectively.

  2. Two half-sandwiched ruthenium (II) compounds containing 5-fluorouracil derivatives: synthesis and study of DNA intercalation.

    Science.gov (United States)

    Li, Zhao-Jun; Hou, Yong; Qin, Da-An; Jin, Zhi-Min; Hu, Mao-Lin

    2015-01-01

    Two novel coordination compounds of half-sandwiched ruthenium(II) containing 2-(5-fluorouracil)-yl-N-(pyridyl)-acetamide were synthesized, and their intercalation binding modes with calf thymus DNA were revealed by hyperchromism of ultraviolet-visible spectroscopy; the binding constants were determined according to a Langmuir adsorption equation that was deduced on the base of careful cyclic voltammetry measurements. The two compounds exhibited DNA intercalation binding activities with the binding constants of 1.13×106 M-1 and 5.35 ×105 M-1, respectively.

  3. SYNTHESIS AND CHARACTERIZATION OF A NEW COMPOUND:K6Ti0.67Nb15.33O42

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    A new compound K6Ti0.67Nb15.33O42 was prepared for the first time by solid state reaction in K2O-Ni2O3-Nb2O5 ternary system.The new compound was characterized by electron probe,X-ray powder diffraction and DTA.The result of X-ray powder diffraction shows that K6Ti0.67Nb15.33O42 crystallizes the hexagonal system with unit cell parameters a=9.1341(5)(),c=12.090(1) (),and space group P63/mcm(193).

  4. Synthesis, Characterization, Crystal Structure and Quantum Chemical Calculation of Novel Compound 1,3-Dimethyl-2-ferrocenylmethylbenzimidazolium Iodide

    Institute of Scientific and Technical Information of China (English)

    ZHANG Jing; YANG Bing-Qin; ZHU Hai-Yan; LI Tao; WEN Zhen-Yi

    2006-01-01

    A novel benzimidazole derivative, 1,3-dimethyl-2-ferrocenylmethylbenzimidazolium iodide (1) was synthesized and characterized by elemental analysis, MS, 1H NMR and IR spectra. Its crystal structure was determined by X-ray single crystal diffraction, and the title compound belongs to monoclinic system with space group P2(1)/c.According to the crystal structure, the quantum chemistry calculation was performed by Gaussian 03 program, and full geometry optimizations of the title compound were carried out with DFT method at B3LYP/6-31G level. Its structure, stability, frontier molecular orbital components and net charge distribution were discussed.

  5. Design, Synthesis and Biological Evaluation of 1,4-Disubstituted-3,4-dihydroisoquinoline Compounds as New Tubulin Polymerization Inhibitors

    Directory of Open Access Journals (Sweden)

    Ling Zhang

    2015-05-01

    Full Text Available A series of 1,4-disubstituted-3,4-dihydroisoquinoline derivatives designed as tubulin polymerization inhibitors were synthesized. Their cytotoxic activities against the CEM leukemia cell line were evaluated. Most of them displayed moderate cytotoxic activities, and compounds 21 and 32 showed good activities with IC50 of 4.10 and 0.64 μM, respectively. The most potent compound 32 was further confirmed to be able to inhibit tubulin polymerization, and its hypothetical binding mode with tubulin was obtained by molecular docking.

  6. Synthesis and in vitro antitumor activity of an isomer of the marine pyridoacridine alkaloid ascididemin and related compounds.

    Science.gov (United States)

    Delfourne, Evelyne; Kiss, Robert; Le Corre, Laurent; Merza, Joumaa; Bastide, Jean; Frydman, Armand; Darro, Francis

    2003-10-01

    The isomer (9H-quino[4,3,2-de][1,7]phenanthroline-9-one) (2) of the marine alkaloid ascididemin (9H-quino[4,3,2-de][1,10]phenanthroline-9-one) (1) has been synthesized in six steps from 1,4-dimethoxyacridine (10) with an overall yield of 12%. Different related compounds were prepared and tested in vitro at six different concentrations on 12 different human cancer cell lines of various histopathological types (glioblastomas and breast, colon, lung, prostate and bladder cancers). Almost all the compounds present cytotoxic activity of micromolar order.

  7. Synthesis of Biological Reports on Juvenile Fish Passage and Survival at Bonneville Dam through 2005

    Energy Technology Data Exchange (ETDEWEB)

    Ploskey, Gene R.; Johnson, Gary E.; Giorgi, Albert E.; Johnson, Richard L.; Stevenson, John R.; Schilt, Carl R.; Johnson, Peter N.; Patterson, Deborah S.

    2005-06-01

    This report describes a review of available literature on juvenile salmonid passage at Bonneville Dam from 1939 through 2005. Studies of interest included project-wide fish-passage efficiency (FPE) studies by radio telemetry and fixed-aspect hydroacoustics, fish survival studies (direct and indirect), FGE studies, powerhouse and unit (by netting, hydroacoustics, and radio telemetry), predation studies in the forebay and tailrace, behavioral studies on forebay approach and egress, and surface-bypass studies. The FPE effort will include a review of available distribution data (horizontal, diel, and vertical) for juvenile salmon. This study does not repeat the results of previous review and synthesis studies but cites them. Where no previous review exists for a subject area, all reports were reviewed and synthesized. The report includes an annotated bibliography summarizing each of the documents reviewed and a DVD disk containing all of the original papers and reports along with an HTML index to the documents.

  8. Synthesis of 1-Bromo-3-methoxy-4-propoxy-5-iodobenzene-A Novel Efficient Process for the Synthesis of Brominated Aromatic Compound

    Institute of Scientific and Technical Information of China (English)

    Hong Xin SHI; Hui LIN; Gérard MANDVILLE

    2004-01-01

    The reaction of aromatic carboxylic acid with oxalyl chloride gives rise to the corres- ponding acid chloride which without purification is treated with the sodium salt of mercapto- pyridine oxide in the presence of 2,2-azo-bisisobutyronitrile (AIBN), radical initiator to give a brominated aromatic compound. After etherification and oxidation, 5-iodovaniline was converted to trisubstituted benzene carboxylic acid which give 1-bromo-3-methoxy-4-propoxy-5-iodo- benzene by this new brominating process with a yield of 74 %.

  9. Reducing Emissions of Volatile Organic Compounds - Final Report - 08/15/1997 - 02/14/2001

    Energy Technology Data Exchange (ETDEWEB)

    Stensel, H. David; Strand, Stuart E.

    2001-03-14

    The overall objective of this research was to determine if the shallow suspended growth reactor (SSGR) could provide sufficient treatment performance of organic and reduced sulfur (TRS) compounds, at 50 C to meet the EPA ''cluster rule'' regulatory limits. The biodegradation of a mixture of organic compounds that could be present in pulp and paper high volume low concentration gas streams was evaluated at 50 C in a bench-scale SSGR. The removal of methanol was followed in particular, and was mathematically modeled to evaluate the effect of process design and operating parameters on methanol removal. Additional tests were performed to obtain mass transfer and biodegradation kinetic parameters for the model. The acclimation of microbial populations capable of degrading TRS compounds from various seed sources was studied in batch reactors at 30 and 50 C. The degradation of TRS compounds in bench-scale SSGR was studied at 20-50 C. Also, the biodegradation kinetic and mass transfer coefficients for alpha-terpinene and gamma-terpinene were studied. Finally, a pilot plant was constructed and operated at Simpson pulp and paper mill in Tacoma, WA.

  10. Compound odontoma involving the four quadrants of the jaws: a case report and review of the literature.

    Science.gov (United States)

    Erdogan, Özgür; Keceli, Onur; Öztunc, Haluk; Evlice, Burcu; Altug, Hasan Ayberk; Günhan, Ömer

    2014-04-01

    Odontomas are the most common odontogenic tumors, representing 70% of all odontogenic tumors. They may present in two specific forms; compound odontoma forms multiple small tooth-like structures, while complex odontoma forms an amorphous calcified mass. In this report, we present a 27-year-old male patient with multiple compound odontoma occupied regions at his jaws. The odontomas involve both alveolar and basal processes of the maxilla and mandible as well as both maxillary sinuses. Converse to conventional recommended treatment, which is surgical excision of the lesion, the management was removal of the lesion and clinical-radiologic followup. The first year's follow-up findings are presented in this case report.

  11. Synthesis, Crystal Structure and Quantum Chemical Investigation of Bis-Schiff Base Compounds Derived from2-phenyl-1,2,3-triazole-4-carboxaldehyde with Diamine

    Institute of Scientific and Technical Information of China (English)

    XIE Ling; LIU Gang; WANG Yan; WANG Ji-De; CHEN Jun-Feng

    2008-01-01

    Two new schiff base N,N'-bis((2-phenyl-2H-1,2,3-triazol-4-yl)methylene)-1,3-pro- panediamine (1) and N,N'-bis((2-phenyl-2H-1,2,3-triazol-4-yl)methylene) -1,4-butanediamine (2) were synthesized by condensation of 2-phenyl-1,2,3-triazole-4-carboxaldehyde with diamine, and characterized by elemental analysis, IR, 1H NMR and MS spectra. Their crystal structures were determined by X-ray single crystal diffraction. Both crystals belong to the monoclinic system, space group P21/c. For compound 1(C21H20N8, Mr=384.45): a = 16.314(3), b =5.7168(11), c = 21.316(4)(A),β= 105.3(2)°,Z = 4, V = 1917.6(7)(A)3, Dc =1.332 g/ cm3, F(000) = 808, μ = 0.086 mm- 1, R = 0.0533 and wR = 0.1460; for compound 2 (C22H22N8, Mr =398.48): a = 8.6156(17), b = 5.2964(11), c = 22.665(5) A, β = 100.54(3)°,Z = 2, V = 1016.8(4)(A)3, Dc = 1.302 g/ cm3, F (000) = 420, μ = 0.083 mm-1, R = 0.0373 and wR = 0.1155. Based on the crystal data, quantum chemistry calculation was performed on the two title compounds by means of Gaussian 98 program. The molecular orbital energies and atomic net charges population were obtained. Furthermore, we analyzed their active atoms. The investigation can serve as a theoretical guide to study the synthesis and activity of the title compounds.

  12. Study on Ionic Organotin Compounds Ⅲ. Synthesis of Five-Coordinated Anionic Tin(Ⅳ) Complexes and Crystal Structure of [ ( i-Pr)2NH2] [ PhSn(μ2-SCH2COO)2

    Institute of Scientific and Technical Information of China (English)

    ZHONG Gui-Yun; SUN Li-Juan; XIE Qing-Lan

    2003-01-01

    @@ The study of ionic organotin compounds is of current attention owing to their diversified molecular structures and wide range of applications, such as biological activities[1 ~3] and as catalysts in organic synthesis. [4] Recently, we synthesized some new ionic organotin compounds by dephenylation reaction. [5] In this paper, we continued to study the reaction of mercaptoacetic acid with phenyltin trichloride in the presence of organic base. The reaction equation was as follows:

  13. Design, Synthesis and Biological Evaluation of Brain-Targeted Thiamine Disulfide Prodrugs of Ampakine Compound LCX001

    Directory of Open Access Journals (Sweden)

    Dian Xiao

    2016-04-01

    Full Text Available Ampakine compounds have been shown to reverse opiate-induced respiratory depression by activation of amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid (AMPA glutamate receptors. However, their pharmacological exploitations are hindered by low blood-brain barrier (BBB permeability and limited brain distribution. Here, we explored whether thiamine disulfide prodrugs with the ability of “lock-in” can be used to solve these problems. A series of thiamine disulfide prodrugs 7a–7f of ampakine compound LCX001 was synthesized and evaluated. The trials in vitro showed that prodrugs 7e, 7d, 7f possessed a certain stability in plasma and quickly decomposed in brain homogenate by the disulfide reductase. In vivo, prodrug 7e decreased the peripheral distribution of LCX001 and significantly increased brain distribution of LCX001 after i.v. administration. This compound showed 2.23- and 3.29-fold greater increases in the AUC0-t and MRT0-t of LCX001 in brain, respectively, than did LCX001 itself. A preliminary pharmacodynamic study indicated that the required molar dose of prodrug 7e was only one eighth that of LCX001 required to achieve the same effect in mice. These findings provide an important reference to evaluate the clinical outlook of ampakine compounds.

  14. Charge migration in dicationic electrophiles and its application to the synthesis of aza-polycyclic aromatic compounds.

    Science.gov (United States)

    Li, Ang; Kindelin, Patrick J; Klumpp, Douglas A

    2006-03-16

    [reaction: see text] Superacid-promoted reactions of dicationic electrophiles have been studied, and the positive charge centers are found to migrate apart in a predictable manner. Using isotopic labeling the charge migration is found in one system to occur through successive deprotonation-reprotonation steps. The charge migration chemistry is the basis for new general synthetic route to aza-polycyclic aromatic compounds.

  15. Synthesis, crystal structure and electrical properties of the new organic-inorganic hybrid compound bis(1-chlorido-4-aminopyridinium) octachlorodiantimoinate

    Science.gov (United States)

    Fersi, Mohamed Amine; Hajji, Rachid; Chaabane, Iskandar; Gargouri, Mohamed

    2017-10-01

    Bis(1-chlorido-4-aminopyridinium) octachlorodiantimoinate has been synthesized and characterized by a single-crystal X-ray diffraction at 296 K and impedance spectroscopy. At room temperature, the title compound is crystallized in the triclinic system (P 1 ̅ space group) with Z = 2 and the following unit cell dimensions: a = 7.919 (1) Å, b = 9.624 (1) Å, c = 17.692 (3) Å, α = 101.81 (1)°, β = 95.12 (1)°and γ = 112.48 (1)°. The crystal structure of the [C10H12Cl2N4]Sb2Cl8 compound is built of two un-equivalent monoprotonated cations [C5H6N2Cl] + and two un-equivalent tetrachloroantimonate (III) anions noted which are [Sb(1)Cl4]- and [Sb(2)Cl4]-. The arrangement of this compound can be described by an alternation of organic and inorganic layers stacked along [010] direction. The cohesion of compound entities is ensured by hydrogen bonding (N-H…. Cl) and Van Der Waals interaction (C-H…. Cl). The temperature dependence of the σdc conductivity exhibits an Arrhenius type behavior described by the following expression σdc T = Aexp(-Ea/kβT). The Ac conductivity and the dielectric loss suggest that the correlated barrier hopping is the appropriate model for the conduction mechanism.

  16. Synthesis and Luminescent Properties of Two New Triphenylamine-based Compounds with Heterocyclic Ring as Conjugation Bridge

    Institute of Scientific and Technical Information of China (English)

    LI,Qian-Qian; DI,Chong-An; YU,Gui; LIU,Yun-Qi; LI,Zhen; QIN,Jin-Gui

    2008-01-01

    Two new "D-π-D" type triphenylamine-based compounds with a heterocyclic ring,furan or thiophene,as a conjugation bridge were synthesized through a normal Wittig reaction which exhibited good thermal stability and strong luminescence.The preliminary light-emitting diode results indicate that they are promising candidates for the practical application.

  17. Mass transfer in the liquid-phase methanol synthesis (LPMeOH)/sup TM/ process: Interim report

    Energy Technology Data Exchange (ETDEWEB)

    Lee, S.; Parameswaran, V.R.; Sawant, A.V.; Ko, M.K.

    1988-04-01

    This report is a sequel to the Interim Report AP-4429 titled /open quote/Research to Support Development of the Liquid Phase Methanol Synthesis Process/close quote/ (LPMEOH/sup TM/ Process). The focus of this report is on the mass transfer characteristics of the process when the reaction is carried out in a stirred slurry reactor. The relevant aspects of mass transfer theory have been explained and supported with extensive experimental data. As such, this report provides the necessary database for scale-up and design of a stirred slurry reactor for liquid-phase methanol synthesis. 17 refs., 35 figs., 12 tabs.

  18. Two new Cu{sup I} compounds with zwitterionic tetrazolate ligand: In situ synthesis, crystal structures, luminescence and photocatalytic properties

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jian-Yong; Xing, Yuan-Yuan; Wang, Qing-Wei [Shanghai Institute of Technology, Shanghai 200235 (China); Zhang, Na, E-mail: nzhang@sit.edu.cn [Shanghai Institute of Technology, Shanghai 200235 (China); Deng, Wei [Shanghai Institute of Technology, Shanghai 200235 (China); Gao, En-Qing [Shanghai Key Laboratory of Green Chemistry and Chemical Processes, Department of Chemistry, East China Normal University, Shanghai 200062 (China)

    2015-12-15

    Two 2D new Cu(I) coordination polymers, namely [Cu{sub 2}(mpTZ){sub 2}Br{sub 2}]·H{sub 2}O (1), and [Cu{sub 2}(mpTZ){sub 2}N{sub 3}]ClO{sub 4} (2) (mpTZ=N-methyl-4-pyridinium tetrazolate) have been synthesized under solvothermal conditions, in which the mpTZ ligands and Cu{sup I} ions were obtained through in situ [2+3] cycloaddition reaction and reduction reaction of Cu{sup II} salts, respectively. Both compounds have been structural characterized by single crystal X-ray diffraction, FT-IR, PXRD and EA. Compound 1 exhibits a 2D neutral coordination network, in which the Cu{sup I} ions are bridged by η{sub 3}−1, 2, 4-tetrazolate into 2D sheet. In compound 2, the Cu{sup I} ions are linked by azide (in µ{sub 3}−1, 1, 3 bridging mode) and tetrazolate (in η{sub 3}−1, 2, 3 bridging mode) anions into 2D positively charged sheet, extended along the bc plane. Both compounds 1 and 2 exhibit intense bluish green luminescence in the solid state. Photocatalytic performances of the two compounds for the degradation of methylene blue (MB) under visible light were also investigated and the MB degradation in the presence of 1 was nearly complete (99%) after 150 min. - Graphical abstract: Two Cu{sup I}CPs have been solvothermally synthesized through the in situ [2+3] cycloaddition and metal reduction reaction. Both compounds exhibit intense luminescence and high photocatalytic degradation under visible light. - Highlights: • Two new Cu{sup I}-based CPs are solvothermally synthesized through in situ [2+3] cycloaddition reaction and metal reduction reaction. • Both compounds exhibit strong luminescence and photocatalytic degradation of methylene blue (MB) under visible light. • The MB degradation in the presence of 1 is nearly complete (99%) after 150 min.

  19. Unusual route for preparation of manganese(II), cobalt(II), zinc(II) and cadmium(II) carbonate compounds: synthesis and spectroscopic characterizations

    Indian Academy of Sciences (India)

    Moamen S Refat; Mohsen M Al-Qahtani

    2011-07-01

    The manganese(II) carbonate, MnCO3.H2O, cobalt(II) carbonate, CoCO3.4H2O, zinc(II) carbonate, ZnCO3 and cadmium(II) carbonate, CdCO3, respectively, were synthesis by a new simple unusual route during the reaction of aqueous solutions of MnX2, CoX2, ZnX2 and CdX2, where (X = Br- and ClO$^{-}_{4}$) with urea at high temperature within ∼ 90°C for 6 h. The infrared spectra of the reaction products clearly indicate the absence of the bands of urea, but show the characteristic bands of ionic carbonate, CO$^{2-}_{3}$. A general mechanism describing the preparation of manganese(II), cobalt(II), zinc(II) and cadmium(II) carbonate compounds are discussed.

  20. 手性三氟甲基胺类化合物的合成与应用%Synthesis and Application of Chiral Trifluoromethyl Amines Compounds

    Institute of Scientific and Technical Information of China (English)

    刘小华; 徐国明; 翁建新; 刘景伟; 张天明

    2016-01-01

    手性三氟甲基胺类化合物是重要的医药、农药中间体。从不同三氟甲基化试剂的角度出发概括了手性三氟甲基胺类化合物的合成,以及指出了其在药物领域的应用。%Chiral trifluoromethyl amine compounds are important intermediates in medicine and pesti-cide. The synthesis of chiral trifluoromethyl amines was summarized from the point of view of different triflu-oromethylating agents, and their applications in the field of pharmaceuticals were pointed out.