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Sample records for containing1-octylpyridinium 1-octyl-2-methylpyridinium or1-octyl-4-methylpyridinium

  1. Pysico-chemical properties of hydrophobic ionic liquids containing1-octylpyridinium, 1-octyl-2-methylpyridinium or1-octyl-4-methylpyridinium cations

    Energy Technology Data Exchange (ETDEWEB)

    Papaiconomou, Nicolas; Salminen, Justin; Lee, Jong-Min; Prausnitz, John M.

    2006-09-15

    This paper reports synthesis of some ionic liquids based on cations 1-octylpyridinium, 1-octyl-2-methylpyridinium or 1-octyl-4-methylpyridinium and anions dicyanamide [N(CN)2]-, bis(trifluoromethylsulfonyl)imide [Tf2N]-, bis(pentafluoroethylsulfonyl)imide [BETI]-, trifluoromethyl sulfonate [TfO]-, nonafluorobutyl sulfonate [NfO]-, tetrafluoroborate [BF4]-, trifluorophenylborate [BF3Ph]- or hexafluoroarsenate [AsF6]-. Melting points, decomposition temperatures, densities, mutual solubilities with water, and viscosities have been measured. Unlike similar ionic liquids containing imidazolium cations, pyridinium ionic liquids studied here are nearly immiscible in water. Viscosities are similar and water content is slightly lower than those for ionic liquids containing imidazolium cations.

  2. 4-[4-(4-Fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-3-yl]-1-methylpyridinium iodide–4-[3-(4-fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-4-yl]-1-methylpyridinium iodide (0.6/0.4

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    Simona Margutti

    2008-01-01

    Full Text Available The crystal structure of the title compound, C16H16FN2O2+·I−, was determined as part of a study of the biological activity of isoxazolone derivatives as p38 mitogen-activated protein kinase (MAPK inhibitors. The X-ray crystal structure of 4-[4-(4-fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-3-yl]-1-methylpyridinium iodide showed the presence of the regioisomer 4-[3-(4-fluorophenyl-2-methyl-5-oxo-2,5-dihydroisoxazol-4-yl]-1-methylpyridinium iodide. The synthesis of the former compound was achieved by reacting 4-(4-fluorophenyl-3-(4-pyridylisoxazol-5(2H-one after treatment with Et3N in dimethylformamide, with iodomethane. The unexpected formation of the regioisomer could be explained by a rearrangement occurring via aziridine of the isoxazolone compound. The regioisomers have site occupancies of 0.632 (4/0.368 (4. The two six members rings make a dihedral angle of 66.8 (2°.

  3. Thermophysical properties of 1-butyl-4-methylpyridinium tetrafluoroborate

    International Nuclear Information System (INIS)

    Safarov, Javid; Kul, Ismail; El-Awady, Waleed A.; Nocke, Jürgen; Shahverdiyev, Astan; Hassel, Egon

    2012-01-01

    Highlights: ► (p, ρ, T) data of 1-butyl-4-methylpyridinium tetrafluoroborate are estimated. ► The measurements were carried out with a vibration-tube densimeter. ► The thermomechanical coefficients were calculated. - Abstract: Thermophysical properties, {(p, ρ, T) at T = (283.15 to 393.15) K, pressures up to p = 100 MPa, and viscosity at T = (283.15 to 373.15) K and p = 0.101 MPa}, of 1-butyl-4-methylpyridinium tetrafluoroborate [b4mpy][BF 4 ] are reported. The measurements were carried out with a recently constructed Anton-Paar DMA HPM vibration-tube densimeter and a fully automated SVM 3000 Anton-Paar rotational Stabinger viscometer. The vibration-tube densimeter was calibrated using double-distilled water, methanol, toluene, and aqueous NaCl solutions. An empirical equation of state for fitting of the (p, ρ, T) data of [b4mpy][BF 4 ] has been developed as a function of pressure and temperature to calculate the thermal properties of the ionic liquid (IL), such as isothermal compressibility, isobaric thermal expansibility, differences in isobaric and isochoric heat capacities, thermal pressure coefficient, and internal pressure. Internal pressure and the temperature coefficient of internal pressure data were used to make conclusions on the molecular characteristics of the IL.

  4. Thermodynamic properties of 1-butyl-3-methylpyridinium tetrafluoroborate

    International Nuclear Information System (INIS)

    Safarov, Javid; Kul, Ismail; El-Awady, Waleed A.; Shahverdiyev, Astan; Hassel, Egon

    2011-01-01

    Highlights: → (p, ρ, T) data of 1-butyl-3-methylpyridinium tetrafluoroborate are estimated. → The measurements were carried out with a vibration-tube densimeter. → The thermomechanical coefficients were calculated. - Abstract: Pressure, density, temperature (p, ρ, T) data of 1-butyl-3-methylpyridinium tetrafluoroborate [C4mpyr][BF 4 ] at T = (283.15 to 393.15) K and pressures up to p = 100 MPa are reported with an estimated experimental relative combined standard uncertainty of Δρ/ρ = ±(0.01 to 0.08)% in density. The measurements were carried out with a newly constructed Anton-Paar DMA HPM vibration-tube densimeter. The system was calibrated using double-distilled water, methanol, toluene and aqueous NaCl solutions. An empirical equation of state for fitting of the (p, ρ, T) data of [C4mpyr][BF 4 ] has been developed as a function of pressure and temperature to calculate the thermal properties of the ionic liquid (IL), such as isothermal compressibility, isobaric thermal expansibility, differences in isobaric and isochoric heat capacities, thermal pressure coefficient and internal pressure. Internal pressure and the temperature coefficient of internal pressure data were used to make conclusions on the molecular characteristics of the IL.

  5. Synthesis and Structural Characterization of 1-[2-(5-Nitro-1H-indol-2-ylphenyl]methylpyridinium Chloride

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    John B. Bremner

    2011-09-01

    Full Text Available In the course of studies on hybrid antibacterials incorporating 2-aryl-5-nitro-1H-indole moieties as potential bacterial NorA efflux pump inhibitors, the compound 1-[2-(5-nitro-1H-indol-2-ylphenyl]methylpyridinium chloride (2 was synthesized and structurally characterized. This pyridinium chloride salt crystallized in the monoclinic space group P21/c with the following unit cell dimensions: a 10.274(3 Å, b 13.101(4 Å, c 13.439(4 Å, b 107.702(7°, V 1723.2(9 Å3, Z (f.u. = 4; R1 = 0.048, and wR2 = 0.13. Of interest in the single crystal X-ray structure is the (intramolecular disposition of the pyridinium plane over the indole heterocyclic residue [interplanar dihedral angle 17.91(4°].

  6. Selective extraction of copper, mercury, silver and palladium ionsfrom water using hydrophobic ionic liquids.

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    Papaiconomou, Nicolas; Lee, Jong-Min; Salminen, Justin; VonStosch, Moritz; Prausnitz, John M.

    2007-06-25

    Extraction of dilute metal ions from water was performed near room temperature with a variety of ionic liquids. Distribution coefficients are reported for fourteen metal ions extracted with ionic liquids containing cations 1-octyl-4-methylpyridinium [4MOPYR]{sup +}, 1-methyl-1-octylpyrrolidinium [MOPYRRO]{sup +} or 1-methyl-1-octylpiperidinium [MOPIP]{sup +}, and anions tetrafluoroborate [BF{sub 4}]{sup +}, trifluoromethyl sulfonate [TfO]{sup +} or nonafluorobutyl sulfonate [NfO]{sup +}. Ionic liquids containing octylpyridinium cations are very good for extracting mercury ions. However, other metal ions were not significantly extracted by any of these ionic liquids. Extractions were also performed with four new task-specific ionic liquids. Such liquids containing a disulfide functional group are efficient and selective for mercury and copper, whereas those containing a nitrile functional group are efficient and selective for silver and palladium.

  7. Inhibition Effect of 1-Butyl-4-Methylpyridinium Tetrafluoroborate on the Corrosion of Copper in Phosphate Solutions

    OpenAIRE

    Scendo, M.; Uznanska, J.

    2011-01-01

    The influence of the concentration of 1-Butyl-4-methylpyridinium tetrafluoroborate (4MBPBF4) as ionic liquid (IL) on the corrosion of copper in 0.5 M P O 4 3 − solutions of pH 2 and 4 was studied. The research involved electrochemical polarization method, and scanning electron microscopy (SEM) technique. The results obtained showed that the inhibition efficiency of corrosion of copper increases with an increase in the concentration of 4MBPBF4 but decreases with increasing temperature. The the...

  8. Identification of metabolites involved in the biodegradation of the ionic liquid 1-butyl-3-methylpyridinium bromide by activated sludge microorganisms.

    Science.gov (United States)

    Pham, Thi Phuong Thuy; Cho, Chul-Woong; Jeon, Che-Ok; Chung, Yun-Jo; Lee, Min-Woo; Yun, Yeoung-Sang

    2009-01-15

    Ionic liquids (ILs) are low melting organic salts that potentially comprise wide application due to their fascinating properties and have emerged as promising "green" replacements for volatile organic solvents. Despite their nonmeasurable vapor pressure, some quantities of ILs will soon be present in effluent discharges since they do have significant solubility in water. Recently, the toxic effects of ILs toward aquatic communities have been intensively investigated, but little information is available concerning the biodegradable properties of these compounds. The objective of this study was to identify the metabolites generated during the biotransformation of 1-butyl-3-methylpyridinium by microorganisms in aerobic activated sludge. The obtained results revealed that the alkylpyridinium salt was metabolized through the sequential oxidization in different positions of the alkyl side chains. High-performance liquid chromatography and mass-spectrometry analyses demonstrated that this biodegradation led to the formation of 1-hydroxybutyl-3-methylpyridinium, 1-(2-hydroxybutal)-3-methylpyridinium, 1-(2-hydroxyethyl)-3-methylpyridinium, and methylpyridine. On the basis of these intermediate products, biodegradation pathways were also suggested. These findings provide the basic information that might be useful for assessing the factors related to the environmental fate and behavior of this commonly used pyridinium IL.

  9. 2-Methylpyridinium/pyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-olates as potent anticonvulsant agents—synthesis and crystal structure

    Energy Technology Data Exchange (ETDEWEB)

    Mangaiyarkarasi, G.; Kalaivani, D., E-mail: kalaivbalaj@yahoo.co.in [Affiliated to Bharathidasan University, Post Graduate and Research Department of Chemistry, Seethalakshmi Ramaswami College, Tiruchirappalli-620 002 (India)

    2013-12-15

    The molecular salt, 2-methylpyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropy-rimidin-4-olate) (I), is prepared from the ethanolic solution of 1-chloro-2,4-dinitrobenzene, pyrimidine-2,4,6-(1H,3H,5H)-trione (barbituric acid) and 2-methylpyridine at room temperature, and the molecular salt, pyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-olate (II), is prepared from the same reactants, by dissolving them in hot DMSO and ethanol mixture at 70°C. The structures of I and II are characterized by visible, IR, {sup 1}H-NMR, {sup 13}C-NMR and elemental analysis and confirmed by single crystal X-ray analysis. Both the salts crystallize in triclinic crystal system with sp. gr. P-bar1. They possess noticeable anticonvulsant activity even at low concentration (25 mg/kg). Acute toxicity studies of these complexes indicate that LD{sub 50} values are greater than 1500 mg/kg and the tested animals do not show any behavioural changes.

  10. 2-Methylpyridinium/pyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-olates as potent anticonvulsant agents—synthesis and crystal structure

    International Nuclear Information System (INIS)

    Mangaiyarkarasi, G.; Kalaivani, D.

    2013-01-01

    The molecular salt, 2-methylpyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropy-rimidin-4-olate) (I), is prepared from the ethanolic solution of 1-chloro-2,4-dinitrobenzene, pyrimidine-2,4,6-(1H,3H,5H)-trione (barbituric acid) and 2-methylpyridine at room temperature, and the molecular salt, pyridinium 5-(2,4-dinitrophenyl)-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-olate (II), is prepared from the same reactants, by dissolving them in hot DMSO and ethanol mixture at 70°C. The structures of I and II are characterized by visible, IR, 1 H-NMR, 13 C-NMR and elemental analysis and confirmed by single crystal X-ray analysis. Both the salts crystallize in triclinic crystal system with sp. gr. P-bar1. They possess noticeable anticonvulsant activity even at low concentration (25 mg/kg). Acute toxicity studies of these complexes indicate that LD 50 values are greater than 1500 mg/kg and the tested animals do not show any behavioural changes

  11. Inhibition Effect of 1-Butyl-4-Methylpyridinium Tetrafluoroborate on the Corrosion of Copper in Phosphate Solutions

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    M. Scendo

    2011-01-01

    Full Text Available The influence of the concentration of 1-Butyl-4-methylpyridinium tetrafluoroborate (4MBPBF4 as ionic liquid (IL on the corrosion of copper in 0.5 M PO43− solutions of pH 2 and 4 was studied. The research involved electrochemical polarization method, and scanning electron microscopy (SEM technique. The results obtained showed that the inhibition efficiency of corrosion of copper increases with an increase in the concentration of 4MBPBF4 but decreases with increasing temperature. The thermodynamic functions of corrosion analysis and adsorptive behavior of 4MBPBF4 were carried out. During the test, the adsorption of the inhibitor on the copper surface in the phosphate solutions was found to obey the Langmuir adsorption isotherm and had a physical mechanism.

  12. Synthesis, Characterization, Tautomeric Structure and Solvatochromic Behavior of Novel 4-(5-Arylazo-2-Hydroxystyryl-1-Methylpyridinium Iodide as Potential Molecular Photoprobe

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    Farag Altalbawy

    2016-12-01

    Full Text Available A novel series of the title compound 4-(5-arylazo-2-hydroxystyryl-1-methylpyridinium iodide 6 has been synthesized via condensation reactions of the arylazosalicylaldehyde derivatives 4a–i with 1-methyl-picolinium iodide 5. The structures of the new arylazo compounds were characterized by 1H NMR, IR, mass spectroscopy, as well as spectral and elemental analyses. The electronic absorption spectra of arylazomerocyanine compounds 6 were measured in different buffer solutions and solvents. The pK′s and pK*′s in both the ground and excited states, respectively, were determined for the series and their correlations with the Hammett equation were examined. The results indicated that the title arylazomerocyanine dyes 6 exist in the azo form 6A in both ground and excited states. The substituent and solvent effects (solvatochromism of the title compound arylazomerocyanine dyes were determined using the Kamlet-Taft equation and subsequently discussed.

  13. Binding-Induced Fluorescence of Serotonin Transporter Ligands: A Spectroscopic and Structural Study of 4-(4-(Dimethylamino)phenyl)-1-methylpyridinium (APP+) and APP+ Analogues

    Science.gov (United States)

    2014-01-01

    The binding-induced fluorescence of 4-(4-(dimethylamino)-phenyl)-1-methylpyridinium (APP+) and two new serotonin transporter (SERT)-binding fluorescent analogues, 1-butyl-4-[4-(1-dimethylamino)phenyl]-pyridinium bromide (BPP+) and 1-methyl-4-[4-(1-piperidinyl)phenyl]-pyridinium (PPP+), has been investigated. Optical spectroscopy reveals that these probes are highly sensitive to their chemical microenvironment, responding to variations in polarity with changes in transition energies and responding to changes in viscosity or rotational freedom with emission enhancements. Molecular docking calculations reveal that the probes are able to access the nonpolar and conformationally restrictive binding pocket of SERT. As a result, the probes exhibit previously not identified binding-induced turn-on emission that is spectroscopically distinct from dyes that have accumulated intracellularly. Thus, binding and transport dynamics of SERT ligands can be resolved both spatially and spectroscopically. PMID:24460204

  14. Growth and characterization of an organic single crystal: 2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide

    Science.gov (United States)

    Senthil, K.; Kalainathan, S.; Ruban Kumar, A.

    Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. 1H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker’s hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal.

  15. Growth and characterization of an organic single crystal: 2-[2-(4-diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide.

    Science.gov (United States)

    Senthil, K; Kalainathan, S; Ruban Kumar, A

    2014-05-05

    Optically transparent crystal of the organic salt DEASI (2-[2-(4-Diethylamino-phenyl)-vinyl]-1-methyl-pyridinium iodide) has been synthesized by using knoevenagel condensation reaction method. The synthesized material has been purified by successfully recrystallization process. Single crystals of DEASI have been grown by slow evaporation technique at room temperature. The solubility of the title material has been determined at different temperature in acetonitrile/methanol mixture. The cell parameters and crystallinity of the title crystal were determined by single crystal XRD. The powder diffraction was carried out to study the reflection plane of the grown crystal and diffraction peaks were indexed. The presence of different functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) analysis. (1)H NMR spectrum was recorded to confirm the presence of hydrogen nuclei in the synthesized material. The optical property of the title crystal was studied by UV-Vis-NIR spectroscopic analysis. The melting point and thermal property of DEASI were studied using TGA/DSC technique. The Vicker's hardness (Hv) was carried out to know the category. The dielectric constant and dielectric loss of the compound decreases with an increase in frequencies. Chemical etching studies showed that the DEASI grows in the two dimensional growth mechanisms. The Kurtz-Perry powder second harmonic generation (SHG) test has done for title crystal. Copyright © 2014 Elsevier B.V. All rights reserved.

  16. Preparation and drug controlled release of porous octyl-dextran microspheres.

    Science.gov (United States)

    Hou, Xin; Liu, Yanfei

    2015-01-01

    In this work, porous octyl-dextran microspheres with excellent properties were prepared by two steps. Firstly, dextran microspheres were synthesized by reversed-phase suspension polymerization. Secondly, octyl-dextran microspheres were prepared by the reaction between dextran microspheres and ethylhexyl glycidyl ether and freezing-drying method. Porous structure of microspheres was formed through the interaction between octyl groups and organic solvents. The structure, morphology, dry density, porosity and equilibrium water content of porous octyl-dextran microspheres were systematically investigated. The octyl content affected the properties of microspheres. The results showed that the dry density of microspheres decreased from 2.35 to 1.21 g/ml, porosity increased from 80.68 to 95.05% with the octyl content increasing from 0.49 to 2.28 mmol/g. Meanwhile, the equilibrium water content presented a peak value (90.18%) when the octyl content was 2.25 mmol/g. Octyl-dextran microspheres showed high capacity. Naturally drug carriers play an important role in drug-delivery systems for their biodegradability, wide raw materials sources and nontoxicity. Doxorubicin (DOX) was used as a drug model to examine the drug-loading capacity of porous octyl-dextran microspheres. The drug-loading efficiency increased with the increase in microspheres/drug ratio, while the encapsulation efficiency decreased. When microspheres/drug mass ratio was 4/1, the drug-loading efficiency and encapsulation efficiency were 10.20 and 51.00%, respectively. The release rate of DOX increased as drug content and porosity increased. In conclusion, porous octyl-dextran microspheres were synthesized successfully and have the potential to serve as an effective delivery system in drug controlled release.

  17. Vapour pressures and osmotic coefficients of binary mixtures of 1-ethyl-3-methylimidazolium ethylsulfate and 1-ethyl-3-methylpyridinium ethylsulfate with alcohols at T = 323.15 K

    International Nuclear Information System (INIS)

    Calvar, Noelia; Gonzalez, Begona; Dominguez, Angeles; Macedo, Eugenia A.

    2009-01-01

    Osmotic coefficients of binary mixtures containing alcohols (ethanol, 1-propanol, and 2-propanol) and the ionic liquids 1-ethyl-3-methylimidazolium ethylsulfate and 1-ethyl-3-methylpyridinium ethylsulfate were determined at T = 323.15 K. Vapour pressure and activity coefficients of the studied systems were calculated from experimental data. The extended Pitzer model modified by Archer, and the modified NRTL model (MNRTL) were used to correlate the experimental data, obtaining standard deviations lower than 0.012 and 0.031, respectively. The mean molal activity coefficients and the excess Gibbs free energy of the studied binary mixtures were calculated from the parameters obtained with the extended Pitzer model of Archer.

  18. Separation of toluene from alkanes using 1-ethyl-3-methylpyridinium ethylsulfate ionic liquid at T = 298.15 K and atmospheric pressure

    International Nuclear Information System (INIS)

    Gonzalez, Emilio J.; Calvar, Noelia; Gonzalez, Begona; Dominguez, Angeles

    2010-01-01

    In this paper, the separation of toluene from aliphatic hydrocarbons (heptane, or octane, or nonane) was analyzed by solvent extraction with 1-ethyl-3-methylpyridinium ethylsulfate ionic liquid, [EMpy][ESO 4 ]. Liquid-liquid equilibrium (LLE) data for the ternary systems {heptane (1) + toluene (2) + [EMpy][ESO 4 ] (3)}, {octane (1) + toluene (2) + [EMpy][ESO 4 ] (3)}, and {nonane (1) + toluene (2) + [EMpy][ESO 4 ] (3)} were obtained by measurements at T = 298.15 K and atmospheric pressure. The selectivity, % removal of aromatic, and solute distribution ratio, obtained from experimental equilibrium results, were used to determine the ability of [EMpy][ESO 4 ] as a solvent. The degree of consistency of the experimental LLE values was ascertained using the Othmer-Tobias and Hand equations. The experimental results for the ternary systems were correlated with the NRTL model. Finally, the results obtained were compared with other ionic liquids and other solvents.

  19. catena-Poly[2-methylpyridinium [tungstate-di-μ-selenido-silver-di-μ-selenido] 2-methylpyridine monosolvate

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    Lu-Jun Zhou

    2013-11-01

    Full Text Available The title compound, {(C6H8N[AgWSe4]·C6H7N}n, consists of anionic [WAgSe4]n chains, 2-methylpyridinium cations and neutral 2-methylpyridine molecules. The Se atoms bridge the Ag and W atoms, forming a polymeric chain extending along the b-axis direction. Both the Ag and W atoms are located on a twofold rotation axis and each metal atom is coordinated by four Se atoms in distorted tetrahedral geometry. In the crystal, the 2-methylpyridinium cation and 2-methylpyridine molecule are linked via N—H...N hydrogen bonding. Weak C—H...Se interactions link the organic components and polymeric anions into a three-dimensional architecture.

  20. Synthesis and antimicrobial activity of guanylhydrazones. Synthesis of 2-(2-methylthio-2-aminovinyl)-1-methylpyridinium iodides and 2-(2-methylthio-2-aminovinyl)-1-methylquinolinium iodides as potential radioprotective and anticancer agents

    International Nuclear Information System (INIS)

    Almassian, B.

    1985-01-01

    The finding of appreciable antileukemic activity in a series of 2-(2-methylthio-2-amino)vinyl-1-methylquinolinium iodides (Foye et al., 1980, 1983) suggested that greater basicity, as compared with the corresponding dithioacetic acids, was contributing to the increase in activity. The addition of a greater degree of basicity in the design of anticancer possibilities in this series was considered worth investigation, particularly in view of the activity of a series of bis(quanylhydrazones) synthesized at Lederle Laboratories. Accordingly, a series of guanylhydrazones of 4-pyridine-,2-pyridine- and 4-quinolinecarboxyaldehydes was synthesized for anticancer as well as antibacterial screening. Also, substitution of additional basic functions in the 2-(2-methylthio-2-amino) vinyl-1-methylquinolinium and pyridinium iodide series has been made. Appreciable antimicrobial activities have been found with both 2-pyridine and 4-quinolinealdehyde guanylhydrazones, as well as with 2-(2-methylthio-2-amino)vinyl-1-methyl-pyridinium iodides. The overall approach to the synthesis of potential anticancer agents in this project is thus to observe the effect of increasing basicity of these compounds on DNA binding and anticancer activity

  1. Phase equilibrium study of the binary systems (N-hexyl-3-methylpyridinium tosylate ionic liquid + water, or organic solvent)

    International Nuclear Information System (INIS)

    Domanska, Urszula; Krolikowski, Marek

    2011-01-01

    Highlights: → Synthesis, DSC, and measurements of phase equilibrium of N-hexyl-3-methylpyridinium tosylate. → Solvents used: water, alcohols, benzene, alkylbenzenes, and aliphatic hydrocarbons. → Correlation with UNIQUAC, Wilson and NRTL models. → Comparison with different tosylate-based ILs. - Abstract: The (solid + liquid) phase equilibrium (SLE) and (liquid + liquid) phase equilibrium (LLE) for the binary systems ionic liquid (IL) N-hexyl-3-methylpyridinium tosylate (p-toluenesulfonate), {([HM 3 Py][TOS] + water, or an alcohol (1-butanol, or 1-hexanol, or 1-octanol, or 1-decanol), or an aromatic hydrocarbon (benzene, toluene, or ethylbenzene, or propylbenzene), or an alkane (n-hexane, n-heptane, n-octane)} have been determined at ambient pressure using a dynamic method. Simple eutectic systems with complete miscibility in the liquid phase were observed for the systems involving water and alcohols. The phase equilibrium diagrams of IL and aromatic or aliphatic hydrocarbons exhibit eutectic systems with immiscibility in the liquid phase with an upper critical solution temperature as for most of the ILs. The correlation of the experimental data has been carried out using the UNIQUAC, Wilson and the non-random two liquid (NRTL) correlation equations. The results reported here have been compared with analogous phase diagrams reported by our group previously for systems containing the tosylate-based ILs.

  2. Oxidative cleavage of the octyl side chain of 1-(3,4-dichlorobenzyl)-5-octylbiguanide (OPB-2045) in rat and dog liver preparations.

    Science.gov (United States)

    Umehara, K; Kudo, S; Hirao, Y; Morita, S; Uchida, M; Odomi, M; Miyamoto, G

    2000-08-01

    The metabolism of 1-(3,4-dichlorobenzyl)-5-octylbiguanide (OPB-2045), a new potent biguanide antiseptic, was investigated using rat and dog liver preparations to elucidate the mechanism of OPB-2045 metabolite formation, in which the octyl side chain is reduced to four, five, or six carbon atoms. Chemical structures of metabolites were characterized by 1H NMR, fast atom bombardment/mass spectrometry, and liquid chromatography/electrospray ionization-tandem mass spectrometry. Three main metabolites were observed during incubation of OPB-2045 with rat liver S9: 2-octanol (M-1), 3-octanol (M-2), and 4-octanol (M-3). In the incubation of OPB-2045 with dog liver S9, eight metabolites were observed, seven of which being M-1, M-2, M-3, 2-octanone (M-4), threo-2,3-octandiol (M-5), erythro-2,3-octandiol (M-6), and 1,2-octandiol (M-7). M-5 and M-6 were further biotransformed to a ketol derivative and C-C bond cleavage metabolite (hexanoic acid derivative), an in vivo end product, in the incubation with dog liver microsomes. The reactions required NADPH as a cofactor and were significantly inhibited by the various inhibitors of cytochrome P450 (i.e., CO, n-octylamine, SKF 525-A, metyrapone, and alpha-naphthoflavone). The results indicate that the degraded products of OPB-2045 are produced by C-C bond cleavage after monohydroxylation, dihydroxylation, and ketol formation at the site of the octyl side chain with possible involvement of cytochrome P450 systems. This aliphatic C-C bond cleavage by sequential oxidative reactions may play an important role in the metabolism of other drugs or endogenous compounds that possess aliphatic chains.

  3. Product study of 1-adamantyl and 1-bicyclo[2.2.2]octyl radicals in hydrocarbon solvents. An unusually large hydrogen isotope effect

    International Nuclear Information System (INIS)

    Engel, P.S.; Chae, W.K.; Baughman, S.A.; Marschke, G.E.; Lewis, E.S.; Timberlake, J.W.; Luedtke, A.E.

    1983-01-01

    1-Adamantyl (ada.) and 1-bicyclo[2.2.2]octyl (bo.) radicals have been generated by photolysis of the corresponding azoalkanes in various hydrocarbon solvents. Both radicals abstract hydrogen readily from saturated hydrocarbons and they add to aromatic rings much faster than tert-butyl. does. Despite its reactivity, ada. is remarkably selective in hydrogen atom abstraction, preferring a benzylic hydrogen 25:1 over a cyclohexane hydrogen. The effect of solvent viscosity indicates that formation of the radical dimers biada and bibo occurs in the solvent cage. The most striking result of this work is a deuterium isotope effect of 25 for hydrogen transfer from cyclohexane to ada. at 65 0 C. Steric compression in the transition state is postulated to cause an unusually large tunnel correction and hence a large k/sub H//k/sub D/. 6 tables

  4. Crystal structure of a second triclinic polymorph of 2-methylpyridinium picrate

    Directory of Open Access Journals (Sweden)

    Jeganathan Gomathi

    2015-11-01

    Full Text Available The title molecular salt, C6H8N+·C6H2N3O7− (systematic name: 2-methylpyridinium 2,4,6-trinitrophenolate, crystallizes with two cations and two anions in the asymmetric unit. In the crystal, the cations are linked to the anions via bifurcated N—H...(O,O hydrogen bonds, generating R12(6 graph-set motifs. Numerous C—H...O hydrogen bonds are observed between these cation–anion pairs, which result in a three-dimensional network. In addition, weak aromatic π–π stacking between the 2-methylpyridinium rings [inter-centroid distance = 3.8334 (19 Å] and very weak stacking [inter-centroid distance = 4.0281 (16 Å] between inversion-related pairs of picrate anions is observed. The title salt is a second triclinic polymorph of the structure (also with Z′ = 2 reported earlier [Anita et al. (2006. Acta Cryst. C62, o567–o570; Chan et al. (2014. CrystEngComm, 16, 4508–4538]. In the title compound, the cations and anions display a chequerboard arrangement when viewed down [100], whereas in the first polymorph, (010 layers of alternating cations and anions are apparent in a [100] view. It is interesting that the unit-cell lengths are almost identical for the two polymorphs, although the inter-axial angles are quite different.

  5. Mixing thermodynamic properties of 1-butyl-4-methylpyridinium tetrafluoroborate [b4mpy][BF{sub 4}] with water and with an alkan-1ol (methanol to pentanol)

    Energy Technology Data Exchange (ETDEWEB)

    Ortega, J. [Laboratorio de Termodinamica y Fisicoquimica de Fluidos, Parque Cientifico-Tecnologico, Campus Universitario de Tafira, Universidad de Las Palmas de Gran Canaria, 35071-Las Palmas de Gran Canaria, Canary Islands (Spain)], E-mail: jortega@dip.ulpgc.es; Vreekamp, R.; Penco, E.; Marrero, E. [Laboratorio de Termodinamica y Fisicoquimica de Fluidos, Parque Cientifico-Tecnologico, Campus Universitario de Tafira, Universidad de Las Palmas de Gran Canaria, 35071-Las Palmas de Gran Canaria, Canary Islands (Spain)

    2008-07-15

    This article presents a study of the behaviour in solution of 1-butyl-4-methylpyridinium tetrafluoroborate [b4mpy][BF{sub 4}] in water and in the first five alkanols of the series methanol to pentan-1-ol. The excess enthalpies, H{sub m}{sup E} and volumes, V{sub m}{sup E} were determined at the temperatures (298.15 and 318.15) K. At these temperatures, the [b4mpy][BF{sub 4}] was completely miscible in water, methanol, and ethanol, but only partially miscible in the other alkanols. A solubility study was carried out and the (liquid + liquid) equilibria of the ([b4mpy][BF{sub 4}] + alkanol) systems were experimentally determined, evaluating zones of complete miscibility and determining the UCST in each case. The mixtures with water gave positive values of H{sub m}{sup E} and V{sub m}{sup E}, being also positive the changes of these quantities with temperature. The mixtures with alkanols gave values of H{sub m}{sup E}>0 and V{sub m}{sup E}<0, and for these binary mixtures (dH{sub m}{sup E}/dT){sub p}>0 and (dV{sub m}{sup E}/dT){sub p}<0. For all cases, results were interpreted and compared with data obtained in mixtures with another isomer [b3mpy][BF{sub 4}]. Excess properties were correlated with a suitable equation and the area and volume parameters were calculated for [b4mpy][BF{sub 4}].

  6. 2-Amino 4-methylpyridinium 3-chlorobenzoate - A phase matchable organic nonlinear optical material for optoelectronics device applications

    Science.gov (United States)

    Babu, B.; Chandrasekaran, J.; Thirumurugan, R.; Anitha, K.; Saravanabhavan, M.

    2017-09-01

    2-Amino 4-methylpyridinium 3-chlorobenzoate (2A4M3CB) was synthesized and good quality single crystals of the size of 8 × 2 × 1.2 mm3 were harvested from methanol by the slow evaporation solution growth technique at ambient temperature. Single crystal XRD reveals that 2A4M3CB crystallized in monoclinic system with the noncentrosymmetric space group P21. The crystalline phases and functional groups of 2A4M3CB have been identified and confirmed through powder X-ray diffraction and Fourier transform infrared (FTIR) studies, respectively. 1H and 13C NMR were recorded to interpret the molecular structure. The optical transmittance window and the lower cutoff wavelength of the 2A4M3CB have been identified by UV-Vis-NIR studies. Thermal and mechanical stability of the 2A4M3CB crystals were explained by TG/DTA and Vickers hardness analysis. Charge transport mechanism and photo response properties were analyzed through dielectric and photoconductivity studies. Powder second harmonic generation (SHG) characteristics and phase matching ability were explored by Kurtz and Perry powder SHG technique.

  7. Synthesis of novel octyl sinapate to enhance antioxidant capacity of rapeseed-linseed oil mixture.

    Science.gov (United States)

    Szydłowska-Czerniak, Aleksandra; Rabiej, Dobrochna; Krzemiński, Marek

    2018-03-01

    Lipophilisation allows the formation of new functionalised antioxidants having beneficial properties compared to natural hydrophilic phenolic acids. Therefore, this work focused on the synthesis of lipophilic antioxidants, such as a new octyl sinapate, octyl caffeate and octyl ferulate using the modified Fischer esterification of selected hydroxycinnamic acids with 1-octanol. The lipophilic octyl sinapate was obtained for the first time with satisfactory yield (83%) after purification by column chromatography. The identity of the synthesised phenolipids was confirmed by chromatographic and spectroscopic analyses. Antioxidant capacity of phenolipids was determined by DPPH (IC 50  = 35.87-52.24 μg mL -1 ) and ABTS (IC 50  = 39.45-48.72 μg mL -1 ) methods and compared with IC 50 values (7.37-35.30 μg mL -1 and 7.55-41.67 μg mL -1 , respectively) for well known antioxidants. The antioxidant capacity of rapeseed-linseed oil enriched with the purified esters was about two to 30 times higher in comparison with a non-supplemented oil. The novel octyl sinapate as well as octyl caffeate and octyl ferulate have antioxidant properties and lipophilic character, therefore they may be added to vegetable oils as potential antioxidants for tackling oxidative processes. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  8. Octyl Phenol Synthesis Using Natural Clays

    Directory of Open Access Journals (Sweden)

    S. Casuscelli

    2000-03-01

    Full Text Available A series of clay minerals, HB, NB and Al-PILC have been studied in the alkylation reactions of 2-octanol with phenol at 180°C, under conditions of alcohol/phenol = 1 (mole ratio and W/FAo °= 64,27 ghmol-1. The selectivity of Al-PILC was 77,12% for octyl phenol and 16,5% for dioctyl phenol.

  9. Synthesis, characterization and metal adsorption properties of the new ion exchanger polymer 3-n-propyl(4-methylpyridinium) silsesquioxane chloride.

    Science.gov (United States)

    Magosso, H A; Panteleimonov, A V; Kholin, Y V; Gushikem, Y

    2006-11-01

    The preparation and anion exchange properties of 3-n-propyl(4-methylpyridinium) silsesquioxane chloride polymer are described. This new polymer was prepared by the sol-gel processing method and is designated as SiPic+Cl-. It is insoluble in water and showed an anion exchange capacity of 1.46x10(-3) mol g-1. The adsorption isotherms of ZnCl2, CdCl2 and HgCl2 were determined from aqueous solutions and the adsorption equilibria simulations fit the model of fixed bidentate centers with the absence of lateral interactions and energetic heterogeneity between them. The metal ions diffuse into the solid solution interface and are dominantly present as MCl2-(4) species for Zn(II), MCl(2-)4 and MCl-3 species for Cd(II) and MCl-3 species for Hg(II).

  10. Separation of benzene from alkanes using 1-ethyl-3-methylpyridinium ethylsulfate ionic liquid at several temperatures and atmospheric pressure: Effect of the size of the aliphatic hydrocarbons

    International Nuclear Information System (INIS)

    Gonzalez, Emilio J.; Calvar, Noelia; Gomez, Elena; Dominguez, Angeles

    2010-01-01

    The ionic liquid 1-ethyl-3-methylpyridinium ethylsulfate, [EMpy][ESO 4 ], was studied for the separation of benzene from aliphatic hydrocarbons (octane or nonane) by solvent extraction through the determination of the (liquid + liquid) equilibrium (LLE) of the ternary systems: {octane (1) + benzene (2) + [EMpy][ESO 4 ] (3)} and {nonane (1) + benzene (2) + [EMpy][ESO 4 ] (3)} at T = (283.15 and 298.15) K and atmospheric pressure. Binodal curves were determined using the 'cloud point' method, and tie-line compositions were obtained by density measurements. The values of selectivity and distribution coefficient, derived from the tie-line data, were used to decide if this ionic liquid can be used as potential solvent for the separation of benzene from aliphatic hydrocarbons using liquid extraction. These results were analyzed and compared to those previously reported for the systems {hexane + benzene + [EMpy][ESO 4 ]} and {heptane + benzene + [EMpy][ESO 4 ]}. The experimental results show that this ionic liquid is suitable for the extraction of benzene from mixtures containing octane and nonane. The consistency of tie-line data was ascertained by applying the Othmer-Tobias and Hand equations. The experimental results for the ternary systems were well correlated with the NRTL model. No literature data were found for the mixtures discussed in this paper.

  11. 1,4,9,12-Tetramethoxy-14-octyl-5,8-dihydrodiindolo[3,2-b;2′,3′-h]carbazole with an unknown solvent

    Directory of Open Access Journals (Sweden)

    Norma Wrobel

    2017-03-01

    Full Text Available The title compound, 2C36H39N3O4·H2O, is a linear π-conjugated ladder oligomer with an alkyl chain on the central nitrogen atom. This diindolocarbazole, prepared via a twofold Cadogan reaction, adopts a sligthly convex shape, anti to the disordered octyl group. The unit cell contains nine molecules of the title compound and half a water molecule per main molecule. The water molecule forms hydrogen bridges, connecting the carbazole-NH and methoxy groups of different molecules. The crystal contains solvent molecules which are located in a channel parallel to the c axis. It was not possible to determine the position and nature of the solvent (a mixure of choroform, n-pentane and DMSO. The SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18] option of PLATON was used to model the missing electron density. The given chemical formula and other crystal data do not take into account these solvent molecules.

  12. Allergic contact dermatitis from 2-n-octyl-4-isothiazolin-3-one, a paint mildewcide

    DEFF Research Database (Denmark)

    Mathias, C G; Andersen, Klaus Ejner; Hamann, K

    1983-01-01

    Severe allergic contact dermatitis from a paint mildewcide, 2-n-octyl-4-isothiazolin-3-one, developed in a worker formulating latex paints within a paint manufacturing company, Guinea pig maximization testing demonstrated this to be a moderate sensitizer. Further cases of allergic contact...... dermatitis may be encountered as the use of this biocide increases in the market place....

  13. Structure, physicochemical and biological properties of an aqua (2,2{sup '},2''-nitrilotriacetato)-oxidovanadium(IV) salt with 4-methylpyridinium cation

    Energy Technology Data Exchange (ETDEWEB)

    Tesmar, Aleksandra; Wyrzykowski, Dariusz; Drzezdzon, Joanna; Jacewicz, Dagmara; Chmurzynski, Lech [Faculty of Chemistry, University of Gdansk (Poland); Kazimierczuk, Katarzyna [Department of Inorganic Chemistry, Gdansk University of Technology (Poland); Klak, Julia [Faculty of Chemistry, Wroclaw University (Poland); Kowalski, Szymon; Inkielewicz-Stepniak, Iwona [Department of Medical Chemistry, Medical University of Gdansk (Poland)

    2017-04-04

    The crystal structure of a nitrilotriacetate (nta) oxidovanadium(IV) salt with 4-methylpyridinium cation, [4-Me(Py)H]{sup +}, of [4-Me(Py)H][VO(nta)(H{sub 2}O)] stoichiometry was determined. The complex comprises a discrete mononuclear [VO(nta)(H{sub 2}O)]{sup -} coordination entity that can be rarely found among other known compounds containing nitrilotriacetate oxidovanadium(IV) moieties. The complex was characterized by spectroscopic (IR and EPR) methods, magnetic measurements, and thermogravimetry (TG-FTIR). The stability of the title compound in aqueous solutions was investigated by using the potentiometric titration method. Furthermore, spectrophotometric (UV/Vis) studies have revealed that the compound is capable to scavenge the superoxide free radicals (O{sub 2} {sup circle} {sup -}) as well as stable organic radicals i.e. 2,2'-azinobis(3-ethylbenzothiazoline-6 sulfonic acid) cation radical (ABTS{sup +} {sup circle}) and 2,2-diphenyl-1-picrylhydrazyl radical (DPPH {sup circle}). Finally, biological properties of the complex studied were investigated in relation to its cytoprotective activity against the oxidative damage generated exogenously by using hydrogen peroxide in the HT22 hippocampal neuronal cell line (the MTT assay). Additionally, the biological action of the compound towards two human osteosarcoma HOS and MG-63 cell lines (the MTT and BrdU tests) as well as the untransformed human osteoblast hFOB 1.19 cell line was tested. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  14. 40 CFR 180.1130 - N-(n-octyl)-2-pyrrolidone and N-(n-dodecyl)-2-pyrrolidone; exemptions from the requirement of a...

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false N-(n-octyl)-2-pyrrolidone and N-(n... EXEMPTIONS FOR PESTICIDE CHEMICAL RESIDUES IN FOOD Exemptions From Tolerances § 180.1130 N-(n-octyl)-2-pyrrolidone and N-(n-dodecyl)-2-pyrrolidone; exemptions from the requirement of a tolerance. N-(n-octyl)-2...

  15. Liquid-liquid phase equilibrium and heat capacity of binary solution {2-propanol + 1-octyl-3-methylimidazolium hexafluorophosphate}

    International Nuclear Information System (INIS)

    Guo, Yimin; Zhang, Xianshuo; Xu, Chen; Shen, Weiguo

    2017-01-01

    Highlights: • Liquid-liquid equilibrium of binary {2-propanol + RTIL} solution was measured. • The critical exponents were deduced and found to belong to 3D-Ising universality. • Asymmetry of the coexistence curve was analyzed by the complete scaling theory. • The dependences of critical parameters on the permittivity of alkanols were discussed. - Abstract: The liquid-liquid coexistence curve and the heat capacity for binary solution of {2-propanol + 1-octyl-3-methylimidazolium hexafluorophosphate} have been precisely measured. The values of the critical exponents α and β, characterizing the critical anomalies of the heat capacity and the coexistence curve respectively, were deduced and found to be consistent with theoretical predictions. The asymmetric behavior of the diameter of the coexistence curve was studied in the frame of the complete scaling theory, demonstrating that the heat capacity related term is of importance. Furthermore, the restricted primitive model (RPM) was used to calculate the reduced upper consolute temperature and density, which together with a comparative larger value of A + indicated a character of solvophobic criticality.

  16. Synthesis and Characterization of Ru(II) Tris(1,1O-phenanthroline)-Electron Acceptor Dyads Incorporating the 4-benzoyl-N-methylpyridinium Cation or N-Benzyl-N'-methyl-viologen. Improving the Dynamic Range, Sensitivity and Response Time of Sol-Gel Based Optical Oxygen Sensors

    Science.gov (United States)

    Leventis, Nicholas; Rawashdeh, Abdel-Monen M.; Elder, Ian A.; Yang, Jinhua; Dass, Amala; Sotiriou-Leventis, Chariklia

    2004-01-01

    The title compounds (1 and 2, above) were synthesized by Sonogashira coupling reactions of appropriate Ru(1I) complexes with the electron a cceptors. Characterization was conducted in solution and in frozen ma trices. Finally, the title compounds were evaluated as dopants of sol-gel materials. It was found that the intramolecular quenching efficie ncy of 4-benzoyl-Nmethylpyridinium cation in solution depends on the solvent: photoluminescence is quenched completely in CH,CN, but not i n methanol or ethanol. On the other hand, intramolecular emission que nching by 4-benzyl-N-methyl viologen is complete in all solvents. The difference between the two quenchers is traced electrochemically to t he solvation of the 4-benzoyl-Nmethylpyridiniums by alcohol. In froze n matrices or adsorbed on the surfaces of silica aerogel, both Ru(I1) complex/electron acceptor dyads of this study are photoluminescent, and the absence of quenching has been traced to the environmental rigi dity. When doped aerogels are cooled at 77 K, the emission intensity increases by approximately 4x, and the spectra shift to the blue, analogous to what is observed with Ru(I1) complexes in solutions undergoi ng fluid-to-rigid transition. However, in contrast to frozen solution s, the luminescent moieties in the bulk of aerogels kept at low tempe ratures are still accessible to gas-phase quenchers diffusing through the mesopores, leading to more sensitive platforms for sensors than o ther room-temperature configurations. Thus the photoluminescence of o ur Ru(I1) complex dyads adsorbed on aerogel is quenchable by O2 both at room temperature and at 77 K. Furthermore, it was also found that O 2 modulates the photoluminescence of aerogels doped with 4-benzoyl -N -methylpyridinium-based dyads over a wider dynamic range compared wi th aerogels doped with either our vislogen-based dyads or with Ru(I1) tris(1,lO-phenanthroline) itself.

  17. Viscometric studies of interactions between ionic liquid 1-octyl-3-methyl-imidazolium bromide and polyvinyl pyrrolidone in aqueous solutions

    International Nuclear Information System (INIS)

    Mehrdad, Abbas; Shekaari, Hemayat; Niknam, Zahra

    2014-01-01

    Highlights: • Viscosities of PVP in aqueous solution of IL are measured. • The flow activation energies are calculated. • The flow activation energies are correlated in terms of polymer concentration. • Intrinsic viscosity of PVP is decreased by increasing temperature. - Abstract: Ionic liquids are investigated as solvents for polymerization processes, as plasticizers of various kinds of polymers and as components of the polymeric matrixes. In this research, viscosity of polyvinyl pyrrolidone in aqueous solution of ionic liquid, 1-octyl-3-methyl imidazolium bromide are measured at various temperatures. The flow activation energies are calculated and correlated in terms of polymer concentration. From sign of the initial slope of the activation energy versus polymer concentration at zero concentration, it is concluded that thermodynamic quality of ionic liquid aqueous solutions are reduced by increasing temperature. The value of the intrinsic viscosity of polyvinyl pyrrolidone was determined using Huggins equation and thermodynamic parameters of this polymer were calculated on the basis of intrinsic viscosity. Also the effect of ionic liquid, 1-octyl-3-methyl imidazolium bromide on the thermodynamic parameters of dilute aqueous polyvinyl pyrrolidone solutions, such as (polymer + solvent) interaction parameter, theta temperature, the heat of dilution parameter and the entropy of dilution parameter was investigated. Results suggest that the thermodynamic quality of water was increased slightly by the addition of ionic liquid in aqueous solution of polyvinyl pyrrolidone

  18. 4-Aminobenzoic acid 4-methylpyridine/4-methylpyridinium 4-aminobenzoate 0.58/0.42: a redetermination from the original data

    Directory of Open Access Journals (Sweden)

    Jan Fábry

    2017-10-01

    Full Text Available The title structure, 4-aminobenzoic acid 4-methylpyridine/4-methylpyridinium 4-aminobenzoate 0.58/0.42, 0.58(C6H7N·C7H7NO2·0.42(C6H8N+·C7H6NO2−, has been redetermined from the data published by Kumar et al. (2015. Acta Cryst. E71, o125-o126. The improvement of the present redetermination consists in the introduction of disorder of the methyl group over two positions as well as in the correction of the positional parameters of the hydrogen atoms that are involved in the O—H...N or N—H...O hydrogen bonds. After the correction, the hydroxyl hydrogen atom turned out to be disordered over two positions about the centre of the O...N bond, which is relatively long [2.642 (2 Å], while the H atoms of the primary amine group account more realistically for the hydrogen-bond pattern after the removal of the positional constraints. All the O—H...N or N—H...O hydrogen bonds which are present in the title structure are of moderate strength.

  19. Light-Emitting Diodes Based on Colloidal Silicon Quantum Dots with Octyl and Phenylpropyl Ligands.

    Science.gov (United States)

    Liu, Xiangkai; Zhao, Shuangyi; Gu, Wei; Zhang, Yuting; Qiao, Xvsheng; Ni, Zhenyi; Pi, Xiaodong; Yang, Deren

    2018-02-14

    Colloidal silicon quantum dots (Si QDs) hold ever-growing promise for the development of novel optoelectronic devices such as light-emitting diodes (LEDs). Although it has been proposed that ligands at the surface of colloidal Si QDs may significantly impact the performance of LEDs based on colloidal Si QDs, little systematic work has been carried out to compare the performance of LEDs that are fabricated using colloidal Si QDs with different ligands. Here, colloidal Si QDs with rather short octyl ligands (Octyl-Si QDs) and phenylpropyl ligands (PhPr-Si QDs) are employed for the fabrication of LEDs. It is found that the optical power density of PhPr-Si QD LEDs is larger than that of Octyl-Si QD LEDs. This is due to the fact that the surface of PhPr-Si QDs is more oxidized and less defective than that of Octyl-Si QDs. Moreover, the benzene rings of phenylpropyl ligands significantly enhance the electron transport of QD LEDs. It is interesting that the external quantum efficiency (EQE) of PhPr-Si QD LEDs is lower than that of Octyl-Si QD LEDs because the benzene rings of phenylpropyl ligands suppress the hole transport of QD LEDs. The unbalance between the electron and hole injection in PhPr-Si QD LEDs is more serious than that in Octyl-Si QD LEDs. The currently obtained highest optical power density of ∼0.64 mW/cm 2 from PhPr-Si QD LEDs and highest EQE of ∼6.2% from Octyl-Si QD LEDs should encourage efforts to further advance the development of high-performance optoelectronic devices based on colloidal Si QDs.

  20. Synthesis and Catalytic Properties of Non-Cross-Linked and Cross-Linked Poly(alkylmethyldiallylammonium bromides) Having Decyl, Octyl, and Hexyl Side Chains

    NARCIS (Netherlands)

    Wang, G.J; Engberts, J.B.F.N.

    1995-01-01

    A family of non-cross-linked and cross-linked copolymers containing decyl, octyl, and hexyl groups as side chains ((CL)-CopolC1-10, (CL)-CopolC1-8, and (CL)-CopolC1-6, respectively) were synthesized by radical-initiated cyclocopolymerization of alkylmethyldiallylammonium bromide monomers without and

  1. All-Polymer Photovoltaic Devices of Poly(3-(4- n -octyl)-phenylthiophene) from Grignard Metathesis (GRIM) Polymerization

    KAUST Repository

    Holcombe, Thomas W.

    2009-10-14

    (Graph Presented) The synthesis of poly[3-(4-n-octyl)-phenylthiophene] (POPT) from Grignard Metathesis (GRIM) is reported. GRIM POPT is found to have favorable electronic, optical, and processing properties for organic photovoltaics (OPVs). Space-charge limited current and field effect transistor measurements for POPT yielded hole mobilities of 1 × 10-4 cm2/(V s) and 0.05 cm2/(V s), respectively. Spincasting GRIM POPT from chlorobenzene yields a thin film with a 1.8 eV band gap, and PC61BM:POPT bulk heterojection devices provide a peak performance of 3.1%. Additionally, an efficiency of 2.0% is achieved in an all-polymer, bilayer OPV using poly[2-methoxy-5-(2′-ethylhexyloxy)-1,4-(1-cyanovinylene) phenylene] (CNPPV) as an acceptor. This state-of-the-art all-polymer device is analyzed in comparison to the analogous poly(3-hexylthiophene) (P3HT)/CNPPV device. Counter to expectations based on more favorable energy level alignment, greater active layer light absorption, and similar hole mobility, P3HT/CNPPV devices perform less well than POPT/CNPPV devices with a peak efficiency of 0.93%. © 2009 American Chemical Society.

  2. All-Polymer Photovoltaic Devices of Poly(3-(4- n -octyl)-phenylthiophene) from Grignard Metathesis (GRIM) Polymerization

    KAUST Repository

    Holcombe, Thomas W.; Woo, Claire H.; Kavulak, David F.J.; Thompson, Barry C.; Fréchet, Jean M. J.

    2009-01-01

    (Graph Presented) The synthesis of poly[3-(4-n-octyl)-phenylthiophene] (POPT) from Grignard Metathesis (GRIM) is reported. GRIM POPT is found to have favorable electronic, optical, and processing properties for organic photovoltaics (OPVs). Space-charge limited current and field effect transistor measurements for POPT yielded hole mobilities of 1 × 10-4 cm2/(V s) and 0.05 cm2/(V s), respectively. Spincasting GRIM POPT from chlorobenzene yields a thin film with a 1.8 eV band gap, and PC61BM:POPT bulk heterojection devices provide a peak performance of 3.1%. Additionally, an efficiency of 2.0% is achieved in an all-polymer, bilayer OPV using poly[2-methoxy-5-(2′-ethylhexyloxy)-1,4-(1-cyanovinylene) phenylene] (CNPPV) as an acceptor. This state-of-the-art all-polymer device is analyzed in comparison to the analogous poly(3-hexylthiophene) (P3HT)/CNPPV device. Counter to expectations based on more favorable energy level alignment, greater active layer light absorption, and similar hole mobility, P3HT/CNPPV devices perform less well than POPT/CNPPV devices with a peak efficiency of 0.93%. © 2009 American Chemical Society.

  3. 2-octyl-cyanoacrylate glue for fixation of STSG in genitourinary tissue defects due to Fournier gangrene: a preliminary trial.

    Science.gov (United States)

    Sivrioğlu, Nazan; Irkören, Saime; Ceylan, Ender; Sonel, Ali Murat; Copçu, Eray

    2013-05-01

    In these reported cases, we observed the outcomes of skin take and wound healing using 2-octyl-cyanoacrylate glue, which was used as tissue glue in the reconstruction of complex genital skin loss due to fournier gangrene. Fifteen patients with Fournier's gangrene were treated in this study. After initial surgical debridement, all defects were repaired using STSG. In this method a thin layer of 2-octyl-cyanoacrylate was dripped on the recipient site immediately before graft application. All wounds were followed up postoperatively and observed for evidence of graft take, seroma or hematoma formation, drainage, and infection. Patient and physician satisfaction were also determined. Grafts were completely accepted in all fifteen patients. None of the patients had wound infection, seroma, hematoma, or other complications. Use of 2-octyl-cyanoacrylate glue (Glueseal) for STSG fixation in complex genital skin defects after Fournier gangrene may be an acceptable alternative to conventional surgical closure with a good cosmetic outcome. Further studies are needed to confirm our initial success with this approach.

  4. Glass transition behavior of octyl β-D-glucoside and octyl β-D-thioglucoside/water binary mixtures.

    Science.gov (United States)

    Ogawa, Shigesaburo; Asakura, Kouichi; Osanai, Shuichi

    2010-11-22

    The lyotropic behavior and glass-forming properties of octyl β-D-glucoside (C8Glu) and octyl β-D-thioglucoside (C8SGlu)/water binary mixtures were evaluated using differential scanning calorimetry (DSC) and polarizing optical microscopy (POM). The results clearly indicate that the mixture forms a glass in the supercooling state of liquid crystalline phases such as cubic, lamellar, and smectic. The glass transition temperature (T(g)) of the mixture was strongly dependent on solute concentration, with a higher concentration correlating with a higher T(g). The experimental T(g) was consistent with the predicted value calculated using the Couchman-Karasz equation in both the C8Glu and C8SGlu/water mixtures. The change of heat capacity at T(g) showed the two bending points under variation of concentrations. And the highest temperature of phase transition from lamellar to isotropic solution was observed at around 50% molar concentration. It was expected that non-percolated state of water existed in extremely higher concentration ranges. Copyright © 2010 Elsevier Ltd. All rights reserved.

  5. Use of 2-octyl cyanoacrylate adhesive in rat liver induced lesion.

    Science.gov (United States)

    Santos, Orlando José dos; Marques, Giancarlo de Souza; Sauaia Filho, Euler Nicolau; Frota, Gustavo Medeiros; Santos, Rayan Haquim Pinheiro; Santos, Rennan Abud Pinheiro

    2012-09-01

    To evaluate the healing process of rat traumatic liver lesion corrected with the use of 2-octyl cyanoacrylate adhesive, compared to the use of biologically absorbable chromed catgut thread suture. Thirty mail adult rats were divided into two groups (15 per group) according to the used method for liver lesion correction as follows: adhesive group (AG), and catgut group (CG); each group being divided into three subsets of five animals (7th, 14th, and 21st day), respectively, according to post-surgery evaluation. All animals were submitted to homogeneous lesion applying synthetic bonding to AG and using chromed catgut suture to CG for lesion correction. Macroscopic and microscopic parameters of healing processes were evaluated. Both groups of animals showed excellent abdominal wall healing, with no evidence of infection, and no abdominal cavity peritonitis or abscess. The presence of adherence was observed in both groups with no statistically significant difference. As to macroscopic evaluation, there was statistically significant difference with respect to specific factors of clinical inflammation (ischemic inflammation and giant celular inflammatory reaction) between animals evaluated on the 10th day (ischemic necrosis and giant cellular inflammatory reaction) among animals evaluated on the 14th day (A14 versus C14). Applying 2-octyl-cyanoacrylate adhesive for correcting rat liver lesion does not change healing process when compared to the use of chromed catgut stitch.

  6. 3-Methylpyridinium 4-nitrobenzoate–4-nitrobenzoic acid (1/1

    Directory of Open Access Journals (Sweden)

    P. Sivakumar

    2016-06-01

    Full Text Available In the title compound, C6H8N+·C7H4NO4−·C7H5NO4, the cation is protonated at its pyridine N atom and makes a dihedral angle of 74.14 (12° with the benzene ring of the anion. The benzene ring of the neutral molecule and the pyridine ring are inclined at an angle of 79.20 (12°. The two benzene rings form a dihedral angle of 6.00 (12° with each other. In the crystal, N—H...O, O—H...O and C—H...O hydrogen bonds link the cations, anions and neutral molecules to form layers parallel to the ac plane, which enlose R44(18 ring motifs. The layers are linked by further C—H...O hydrogen bonds and C—H...π interactions, forming a three-dimensional supramolecular architecture.

  7. n-Octyl gallate as inhibitor of pyruvate carboxylation and lactate gluconeogenesis.

    Science.gov (United States)

    Eler, Gabrielle Jacklin; Santos, Israel Souza; de Moraes, Amarilis Giaretta; Comar, Jurandir Fernando; Peralta, Rosane Marina; Bracht, Adelar

    2015-04-01

    The alkyl gallates are found in several natural and industrial products. In the latter products, these compounds are added mainly for preventing oxidation. In the present work, the potencies of methyl gallate, n-propyl gallate, n-pentyl gallate, and n-octyl gallate as inhibitors of pyruvate carboxylation and lactate gluconeogenesis were evaluated. Experiments were done with isolated mitochondria and the isolated perfused rat liver. The potency of the gallic acid esters as inhibitors of pyruvate carboxylation in isolated mitochondria obeyed the following decreasing sequence: n-octyl gallate > n-pentyl gallate > n-propyl gallate > methyl gallate. A similar sequence of decreasing potency for lactate gluconeogenesis inhibition in the perfused liver was found in terms of the portal venous concentration. Both actions correlate with the lipophilicity of the compounds. The effects are harmful at high concentrations. At appropriate concentrations, however, octyl gallate should act therapeutically because its inhibitory action on gluconeogenesis will contribute further to its proposed antihyperglycemic effects. © 2014 Wiley Periodicals, Inc.

  8. Electrochemical studies of UO22+ in 1-octyl 3- methylimidazolium hexafluorophosphate (omimPF6) room temperature ionic liquid

    International Nuclear Information System (INIS)

    Kamat, J.V.; Gopinath, N.; Lohithakshan, K.V.; Aggarwal, S.K.

    2007-01-01

    The effect of the degraded products on the Electrochemical Window (EW) of l-octyl 3- methylimidazolium hexafluorophosphate (OmimPF 6 ) were studied. Studies were also carried to optimize conditions for extraction of UO 2 2+ to investigate its redox behavior in OmimPF6 and determine the number of electrons involved in the redox chemistry. The Chronoamperometric technique of evaluating n without knowing diffusion coefficient, D, was devised by Kakihana et al. and has been applied in the present work. The number of electrons involved was determined from the values of slope and intercept of the Cottrell plot. The results of these studies are presented in this paper

  9. Crystal structure of 4-{2-[4-(dimethylaminophenyl]diazen-1-yl}-1-methylpyridinium iodide

    Directory of Open Access Journals (Sweden)

    Katherine Chulvi

    2015-12-01

    Full Text Available The molecular geometry of the ionic title compound, C14H17N4+·I− or DAZOP+·I−, is essentially featureless. Regarding the crystal structure, in addition to the obvious cation–anion Coulombic interactions, the packing is mostly directed by non-covalent interactions involving both ring systems, as well as the iodide anion. It consists of cationic molecules aligned along [101] and disposed in an antiparallel fashion while linked into π-bonded dimeric entities by a stacking contact involving symmetry-related phenyl rings, with a centroid–centroid distance of 3.468 (3 Å and a slippage of 0.951 Å. The dimers are, in addition, sustained by a number of C—H...I and I...π (I...centroid = 3.876 Å interactions involving the anion. Finally, interdimeric contacts are of the C—H...I and C—H...π types.

  10. Removal of malachite green dye from aqueous solution using mesoporous silica synthesized from 1-octyl-3-methylimidazolium chloride ionic liquid

    International Nuclear Information System (INIS)

    Ekka, Basanti; Nayak, Soumitra Ranjan; Dash, Priyabrat; Patel, Raj Kishore

    2016-01-01

    In this research, mesoporous silica was synthesized via a modified sol-gel route using 1-octyl-3-methylimidazolium chloride and was employed to remove malachite green (MG) dye from aqueous solution. Subsequently, this material was characterized and identified by different techniques such as Fourier transform infrared spectroscopy (FT-IR), N_2 adsorption-desorption method, scanning electron microscopy (SEM), and thermosgravimetric analysis (TGA). Unique properties such as high surface area and pore diameter, in addition to highly reactive atoms and presence of various functional groups make the mesoporous silica possible for efficient removal of malachite green (MG). In batch experimental set-up, optimum conditions for quantitative removal of MG by mesoporous silica was attained by varying different variables such as adsorbent dosage, initial dye concentration, contact time, and pH. Optimum values were set as pH of 8.0, 0.5 g of adsorbent at contact time of 120 min. The adsorption of MG follows the pseudo-second-order rate equation. Equilibrium data fitted well with the Freundlich model at all amount of adsorbent, while maximum adsorption capacity was 5.981 mg g"−1 for 0.5 g mesoporous silica synthesized in IL.

  11. Morphological studies of DHSA/ DHSA-Octyl ester/ RBD palm kernel olein/ medium chain triglycerides system

    International Nuclear Information System (INIS)

    Anuar Kassim; Nadarajan, Rathidevi; Mohd Zaizi Desa; Atan Mohd Sharif; Dzulkefly Kuang; Mohd Jelas Haron

    2007-01-01

    Dihydroxystearic acid (DHSA) and octyl dihydroxystearate (DHSA-octyl ester) have been previously prepared from palm oleic acid and preliminary results showed that these compounds are suitable in personal care and cosmetics products. The objective of this research is to study the phase behavior in ternary system of DHSA/DHSA-octyl ester/RBD Palm Kernel Olein (RBDPKOo) and MCT at 85 degree Celsius. From the ternary phase diagram, results showed that all ratios of were completely in two-phase region with various concentrations of RBDPKOo and MCT. The phase changes were observed through polarizing light while the formation of texture was confirmed using polarizing microscope combination with heating. Needles and spherulite textures were found in this system. (author)

  12. Microbial corrosion resistance of galvanized coatings with 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one as a biocidal ingredient in electrolytes

    International Nuclear Information System (INIS)

    Zhai, Xiaofan; Myamina, Maria; Duan, Jizhou; Hou, Baorong

    2013-01-01

    Highlights: •Addition of DCOIT to zinc electrolyte increases current efficiency. •Zn deposited from electrolytes with DCOIT inhibits growth and metabolism of SRB. •DCOIT on coating surfaces influences the coating structure and morphology. •EIS and polarization results show good microbial-corrosion resistance in SRB. -- Abstract: Electrodeposition of galvanized coatings from electrolyte containing 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) can increase microbial corrosion resistance. Coatings were found to inhibit the growth and metabolism of sulphate-reducing bacteria (SRB). Open circuit potentials and corrosion rates of coupons revealed DCOIT effectively influences the coating property. Energy diffraction spectrum and infrared absorption spectra were used to detect DCOIT on the coating surface. Scanning electron microscopy and X-ray diffraction revealed morphological and structural modifications. Electrochemical impedance spectroscopy and polarization techniques determined the corrosion behaviour of coatings in SRB. Results showed coatings formed from electrolytes with DCOIT have improved microbial corrosion resistance and bactericidal action

  13. A kinetic study on the Novozyme 435-catalyzed esterification of free fatty acids with octanol to produce octyl esters.

    Science.gov (United States)

    Chowdhury, Avisha; Mitra, Debarati

    2015-01-01

    Octyl esters can serve as an important class of biolubricant components replacing their mineral oil counterparts. The purpose of the current work was to investigate the enzymatic esterification reaction of free fatty acids (FFA, from waste cooking oil) with octanol in a solvent-free system using a commercial lipase Novozyme 435. It was found that the esterificaton reaction followed the Ping-pong bi-bi kinetics with no inhibition by substrates or products within the studied concentration range. The maximum reaction rate was estimated to be 0.041 mol L(-1) g(-1) h(-1) . Additionally, the stability of Novozyme 435 in the current reaction system was studied by determining its activity and final conversion of FFA to esters after 12 successive utilizations. Novozyme 435 exhibited almost 100% enzyme activity up to 7 cycles of reaction and gradually decreased (by 5%) thereafter. The kinetic parameters evaluated from the study shall assist in the design of reactors for large-scale production of octyl esters from a cheap biomass source. The enzyme reusability data can further facilitate mass production by curtailing the cost of expensive enzyme consumption. © 2015 American Institute of Chemical Engineers.

  14. 2-Amino-4-methylpyridinium 2-hydroxybenzoate

    Directory of Open Access Journals (Sweden)

    Madhukar Hemamalini

    2010-08-01

    Full Text Available The asymmetric unit of the title molecular salt, C6H9N2+·C7H5O3−, contains two cations and two anions. Both the salicylate anions contain an intramolecular O—H...O hydrogen bond, which generates an S(6 ring. Both the 2-amino-4-methylpyridine molecules are protonated at their pyridine N atoms. In the crystal, both cations form two N—H...O hydrogen bonds to their adjacent anions, forming ion pairs. Further N—H...O links generate sheets lying parallel to the ab plane. In addition, weak C—H...O bonds and aromatic π–π stacking interactions [centroid–centroid distances = 3.5691 (9 and 3.6215 (9 Å] are observed between the cations and anions.

  15. Pyridinium based ionic liquids. N-Butyl-3-methyl-pyridinium dicyanoamide: Thermochemical measurement and first-principles calculations

    International Nuclear Information System (INIS)

    Emel'yanenko, Vladimir N.; Verevkin, Sergey P.; Heintz, Andreas

    2011-01-01

    The standard molar enthalpy of formation Δ f H m o (l) of the ionic liquid N-butyl-3-methylpyridinium dicyanamide has been determined at 298.15 K by means of combustion calorimetry. Vaporization of the ionic liquid into the nitrogen stream in order to obtain vaporization enthalpy has been attempted, but no vaporization was achieved. First-principles calculations of the enthalpy of formation in the gaseous phase have been performed for the ionic species using the G3MP2 theory. The combination of traditional combustion calorimetry with modern high-level quantum-chemical calculations allows estimation of the molar enthalpy of vaporization of the ionic liquid under study.

  16. Studies on the growth aspects, structural, thermal, dielectric and third order nonlinear optical properties of solution grown 4-methylpyridinium p-nitrophenolate single crystal

    Science.gov (United States)

    Devi, S. Reena; Kalaiyarasi, S.; Zahid, I. MD.; Kumar, R. Mohan

    2016-11-01

    An ionic organic optical crystal of 4-methylpyridinium p-nitrophenolate was grown from methanol by slow evaporation method at ambient temperature. Powder and single crystal X-ray diffraction studies revealed the crystal system and its crystalline perfection. The rocking curve recorded from HRXRD study confirmed the crystal quality. FTIR spectral analysis confirmed the functional groups present in the title compound. UV-visible spectral study revealed the optical window and band gap of grown crystal. The thermal, electrical and surface laser damage threshold properties of harvested crystal were examined by using TGA/DTA, LCR/Impedance Analyzer and Nd:YAG laser system respectively. The third order nonlinear optical property of grown crystal was elucidated by Z-scan technique.

  17. Crystal structure of 2-cyano-1-methylpyridinium perchlorate

    Directory of Open Access Journals (Sweden)

    Vu D. Nguyen

    2015-11-01

    Full Text Available The asymmetric unit of the title salt, C7H7N2+·ClO4−, comprises two independent formula units. The solid-state structure comprises corrugated layers of cations and of anions, approximately parallel to (010. The supramolecular layers are stabilized and connected by C—H...O hydrogen bonding to consolidate a three-dimensional architecture. A close pyridinium–perchlorate N...O contact [2.867 (5 Å] is noted. The crystal was refined as an inversion twin.

  18. TRU decontamination of high-level Purex waste by solvent extraction using a mixed octyl(phenyl)-N,N-diisobutyl-carbamoylmethylphosphine oxide/TBP/NPH (TRUEX) solvent

    International Nuclear Information System (INIS)

    Horwitz, E.P.; Kalina, D.G.; Diamond, H.; Kaplan, L.; Vandegrift, G.F.; Leonard, R.A.; Steindler, M.J.; Schulz, W.W.

    1984-01-01

    The TRUEX (transuranium extraction) process was tested on a simulated high-level dissolved sludge waste (DSW). A batch counter-current extraction mode was used for seven extraction and three scrub stages. One additional extraction stage and two scrub stages and all strip stages were performed by batch extraction. The TRUEX solvent consisted of 0.20 M octyl(phenyl)-N,N-diisobutylcarbamoyl-methylphosphine oxide-1.4 M TBP in Conoco (C 12 -C 14 ). The feed solution was 1.0 M in HNO 3 , 0.3 M in H 2 C 2 O 4 and contained mixed (stable) fission products, U, Np, Pu, and Am, and a number of inert constituents, e.g., Fe and Al. The test showed that the process is capable of reducing the TRU concentration in the DSW by a factor of 4 x 10 4 (to <100 nCi/g of disposed form) and reducing the quantity of TRU waste by two orders of magnitude

  19. Time-resolved studies of energy transfer from meso-tetrakis(N-methylpyridinium-4-yl)- porphyrin to 3,3'-diethyl-2,2'-thiatricarbocyanine iodide along deoxyribonucleic acid Chain.

    Science.gov (United States)

    Kakiuchi, Toshifumi; Ito, Fuyuki; Nagamura, Toshihiko

    2008-04-03

    The excitation energy transfer from meso-tetrakis(N-methylpyridinium-4-yl)porphyrin (TMPyP) to 3,3'-diethyl-2,2'-thiatricarbocyanine iodide (DTTCI) along the deoxyribonucleic acid (DNA) double strand was investigated by the steady-state absorption and fluorescence measurements and time-resolved fluorescence measurements. The steady-state fluorescence spectra showed that the near-infrared fluorescence of DTTCI was strongly enhanced up to 86 times due to the energy transfer from the excited TMPyP molecule in DNA buffer solution. Furthermore, we elucidated the mechanism of fluorescence quenching and enhancement by the direct observation of energy transfer using the time-resolved measurements. The fluorescence quenching of TMPyP chiefly consists of a static component due to the formation of complex and dynamic components due to the excitation energy transfer. In a heterogeneous one-dimensional system such as a DNA chain, it was proved that the energy transfer process only carries out within the critical distance based on the Förster theory and within a threshold value estimated from the modified Stern-Volmer equation. The present results showed that DNA chain is one of the most powerful tools for nanoassemblies and will give a novel concepts of material design.

  20. Solubility, density and excess molar volume of binary mixtures of aromatic compounds and common ionic liquids at T=283.15K and atmospheric pressure

    OpenAIRE

    Emilio J Gonzalez; Patricia Requejo; Filipa Maia; Ángeles Dominguez; Maria Eugénia Macedo

    2015-01-01

    In this work, the solubility of aromatic compounds (benzene, or toluene, or ethylbenzene, or o-xylene, or m-xylene, or p-xylene) in several ionic liquids (1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, or 1-hexyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide, or 1-ethyl-3-methylpyridinium bis(trifluoromethylsulfonyl)imide, or 1-propyl-3-methylpyridinium bis(trifluoromethylsulfonyl)imide, or 1-ethyl-3-methylpyridinium ethylsulfate, or 1-hexyl-3-methylimidazolium dicyana...

  1. Enhanced CO2 capture in binary mixtures of 1-alkyl-3-methylimidazolium tricyanomethanide ionic liquids with water

    NARCIS (Netherlands)

    Romanos, G.E.; Zubeir, L.F.; Likodimos, V.; Falaras, P.; Kroon, M.C.; Iliev, B.; Adamova, G.; Schubert, T.J.S.

    2013-01-01

    The absorption of carbon dioxide and water in the 1-butyl-3-methylimidazoliun tricyanomethanide ([C4C1im][TCM]) and 1-octyl-3-methylimidazolium tricyanomethanide ([C8C1im][TCM]) ionic liquids (ILs) was systematically investigated for the first time as a function of the H2O content by means of a

  2. Anion influence on thermophysical properties of ionic liquids: 1-butylpyridinium tetrafluoroborate and 1-butylpyridinium triflate.

    Science.gov (United States)

    Bandrés, Isabel; Royo, Félix M; Gascón, Ignacio; Castro, Miguel; Lafuente, Carlos

    2010-03-18

    The thermophysical properties of two pyridinium-based ionic liquids, 1-butylpyridinium tetrafluoroborate and 1-butylpyridinium triflate, have been measured. Thus, densities, refractive indices, speeds of sound, viscosities, surface tensions, isobaric molar heat capacities, and thermal properties have been experimentally determined over a wide range of temperatures. The comparison of the properties of the two ionic liquids has allowed us to analyze in detail the anion influence. Moreover, useful derived properties have been calculated from the results. On the other hand, the influence of the lack of a substituent in the cation has been evaluated when properties of 1-butylpyridinium tetrafluoroborate have been contrasted to those of 1-butyl-n-methylpyridinium tetrafluoroborate, (n = 2, 3, or 4). The study has been carried out paying special attention to interactions between ions in order to elucidate the desired relationship between properties and structural characteristics of ionic liquids.

  3. Physical properties of aqueous mixtures of the ionic 1-ethl-3-methyl imidazolium octyl sulfate: A new ionic rigid gel

    International Nuclear Information System (INIS)

    Cabeza, O.; Vila, J.; Rilo, E.; Domínguez-Pérez, M.; Otero-Cernadas, L.; López-Lago, E.; Méndez-Morales, T.; Varela, L.M.

    2014-01-01

    Graphical abstract: Phase diagram indicating three transitions temperatures: (liquid + gel) (dot symbols), (liquid + crystal) (square symbols) and (crystal + liquid) (triangle symbols) for the aqueous EMIM-OS mixtures. - Highlights: • We present the phase diagram of the system EMIM-octyl sulfate + water. • We show that a rigid gel phase appears for certain concentrations and temperatures. • That gel presents a smectic-like phase, being really a rigid gel crystal. • The gel is as electrical conductive as the liquid in spite of the viscosity change. • Density does not change at the (liquid + gel) transition. - Abstract: We report the existence of hydrophobically driven lyotropic rigid gel phase in aqueous mixtures of the ionic liquid (IL) 1-ethyl-3-methyl imidazolium octyl sulfate (EMIM-OS), and we characterize the physical properties of the gel phase by means of density, electrical conductivity and viscosity measurements. Also we include polarized microscopy images, showing the existence of a crystalline-like gel phase with the cations and anions (mainly the alkyl chain of this last ones) ordered in a fashion similar to a liquid crystal, which is induced by the presence of the water molecules. As was pointed out briefly in a previous paper, some of the mixtures of that system under goes a (liquid + gel) phase transition only in a quite narrow concentration interval: for ionic liquid molar fraction, x IL , from 0.09 to 0.5. Below x IL = 0.09 and above x IL = 0.5, the mixtures crystallize at low temperature becoming a hard solid crystal. Here we report the complete phase diagram of this binary system, as well as measurements of the temperature behavior of several physical properties around the (liquid + gel) and (liquid + crystal) transitions. Curiously enough, we did not detect any change in the temperature dependence of the measured magnitudes at the (liquid + gel) phase transition, but for viscosity, even in the case of the electrical conductivity

  4. In vivo and in vitro evaluation of octyl methoxycinnamate liposomes

    Directory of Open Access Journals (Sweden)

    de Carvalho Varjão Mota A

    2013-12-01

    Full Text Available Aline de Carvalho Varjão Mota,1 Zaida Maria Faria de Freitas,1 Eduardo Ricci Júnior,1 Gisela Maria Dellamora-Ortiz,1 Ralph Santos-Oliveira,2 Rafael Antonio Ozzetti,3 André Luiz Vergnanini,3 Vanessa Lira Ribeiro,4 Ronald Santos Silva,4 Elisabete Pereira dos Santos11Faculty of Pharmacy, Federal University of Rio de Janeiro, 2Nuclear Engineering Institute, National Nuclear Energy Commission, 3Allergisa Dermatocosmetic Research, University of Campinas, São Paulo, 4Pharmacology and Toxicology Department, National Insitute of Quality Control in Health, Oswaldo Cruz Foundation, Rio de Janeiro, BrazilAbstract: Solar radiation causes damage to human skin, and photoprotection is the main way to prevent these harmful effects. The development of sunscreen formulations containing nanosystems is of great interest in the pharmaceutical and cosmetic industries because of the many potential benefits. This study aimed to develop and evaluate an octyl methoxycinnamate (OMC liposomal nanosystem (liposome/OMC to obtain a sunscreen formulation with improved safety and efficacy by retaining OMC for longer on the stratum corneum.Methods: The liposome/OMC nanostructure obtained was tested for enzymatic hydrolysis with lipase from Rhizomucor miehei and biodistribution with liposomes labeled with technetium-99m. The liposome/OMC formulation was then incorporated in a gel formulation and tested for ocular irritation using the hen’s egg test-chorio-allantoic membrane (HET-CAM assay, in vitro and in vivo sun protection factor, in vitro release profile, skin biometrics, and in vivo tape stripping.Results: The liposome/OMC nanosystem was not hydrolyzed from R. miehei by lipase. In the biodistribution assay, the liposome/OMC formulation labeled with technetium-99m had mainly deposited in the skin, while for OMC the main organ was the liver, showing that the liposome had higher affinity for the skin than OMC. The liposome/OMC formulation was classified as nonirritating in

  5. Biochemical and genetic toxicity of the ionic liquid 1-octyl-3-methylimidazolium chloride on earthworms (Eisenia fetida).

    Science.gov (United States)

    Guo, Yingying; Liu, Tong; Zhang, Jun; Wang, Jinhua; Wang, Jun; Zhu, Lusheng; Yang, Jinhui

    2016-02-01

    Ionic liquids also known as "green solvents," are used in many fields. However, the dispersion of ionic liquids in soil systems is likely to cause damage to soil organisms. The objective of the present study was to investigate the toxicity of 1-octyl-3-methylimidazolium chloride ([C8 mim]Cl) on earthworms (Eisenia fetida). For this purpose, earthworms were exposed to different concentrations of [C8 mim]Cl (0 mg/kg, 5 mg/kg, 10 mg/kg, 20 mg/kg, and 40 mg/kg artificial soil) and sampled at 7 d, 14 d, 21 d, and 28 d. The results indicated that [C8 mim]Cl could cause an accumulation of reactive oxygen species (ROS) in earthworms, even at the lowest concentration (5 mg/kg). Compared with the controls, during the [C8 mim]Cl exposure period, the activities of superoxide dismutase (SOD) and catalase (CAT) decreased and then increased, whereas the activities of peroxidase (POD) and glutathione S-transferase (GST) increased. These changes in the activities of antioxidant enzymes and GST indicated that [C8 mim]Cl could induce oxidative damage in earthworms. The malondialdehyde content was increased by high levels of [C8 mim]Cl at 14 d and 28 d, indicating that [C8 mim]Cl could lead to lipid peroxidation in earthworms. In addition, the degree of DNA damage significantly increased with increasing [C8 mim]Cl concentrations and exposure time. The present study shows that [C8 mim]Cl caused biochemical and genetic toxicity in earthworms. © 2015 SETAC.

  6. Fluorescence spectroscopic study of the aggregation behavior of non-cross-linked and cross-linked poly(alkylmethyldiallylammonium bromides) having decyl, octyl, and hexyl side chains in aqueous solution

    NARCIS (Netherlands)

    Wang, G.J; Engberts, J.B.F.N.

    1996-01-01

    The conformational state of a series of non-cross-linked and cross-linked poly(alkylmethyldiallylammonium bromides) bearing decyl, octyl, and hexyl side chains ((CL)-CopolC1-10, (CL)-CopolC1-8, and (CL)-CopolC1-6, respectively) in aqueous solutions were investigated by fluorescence spectroscopy

  7. Acute toxicity of 5-(furan-2-yl, 2-metylfuran-3-yl-4-amino-1,2,4-triazole-3-thiol alkyl derivatives

    Directory of Open Access Journals (Sweden)

    D. M. Danilchenko

    2017-09-01

    Full Text Available The purpose of our work was the further exploration of the new 5-(furan-2-yl, 2-metylfuran-3-yl-4-amino-1,2,4-triazole-3-thiol alkyl derivatives’ acute toxicity, setting some patterns of alkyl substituents influence by the Sulfur atom on the acute toxicity. Research materials and methods. In this study we used first time synthesized 5-(furan-2-yl, 2-metylfuran-3-yl-4-amino-4H-1,2,4-triazole-3-thione derivatives. Acute toxicity was conducted on white rats weighing 160–250 g, which were injected once intraperitoneally with the investigated substances. The rats were received from the nursery of the Pharmacology and Toxicology Institute of Ukraine Medical Sciences Academy. The animals were kept on a standard diet with natural light mode "day-night". Results and their discussion. After the acute toxicity studies in a group of 5-(furan-2-yl, 2-metylfuran-3-yl-4-amino-4H-1,2,4-triazole 3-alkyl derivatives it was found that among all studied structures the most toxic was 2e, LD50 of which was 263 mg/kg, and the least toxic compound was 2a, LD50 of which was 1570 mg/kg, that belongs to the V toxicity class. After comparing the acute toxicity of well-known antimycotic agent fluconazole with the studied compounds it can be argued that most compounds are less toxic than the comparison drug fluconazole with the index of LD50 ˃320 mg/kg. It was found that the transition in a group from butyl to decyl, octyl, ventyl, propyl, nonyl and heptyl substituents in the molecule of 3-alkylthio 5-(furan-2-yl-4-amino-4H-1,2,4-triazole is accompanied by the toxicity increasing. Speaking about the 5-(2-metylfuran-3-yl-4-amino-4H-1,2,4-triazole 3-alkylthio derivatives we can find that this dependence is observed in a number from propyl, pentyl, nonil, butyl, heksyl, octyl and heptyl hydrocarbon chains. Conclusions. The investigated 3-alkylthio 5-(furan-2-yl, 2-metylfuran-3-yl-4-amino-4H-1,2,4-triazole derivatives belong to the IV-V toxicity class. The toxicity of 5

  8. N-mercapto acetyl-N'-octyl-O, N″-glycol chitosan as an efficiency oral delivery system of paclitaxel.

    Science.gov (United States)

    Huo, Meirong; Fu, Ying; Liu, Yanhong; Chen, Qinyu; Mu, Yan; Zhou, Jianping; Li, Lingchao; Xu, Wei; Yin, Tingjie

    2018-02-01

    Herein, thioglycolic acid modified N-octyl-O, N'-glycol chitosan (N-mercapto acetyl-N'-octyl-O, N″-glycol chitosan, abbreviated as SH-OGC) was synthesized to improve the oral bioavailability of paclitaxel (PTX). PTX was readily solubilized into the hydrophobic inner core of SH-OGC. Pharmacokinetic studies demonstrated that the bioavailability of PTX was greatly enhanced when delivered by SH-OGC compared to Taxol ® or non-sulfhydrylated OGC micelles. Caco-2 cell experiments confirmed PTX or rhodamine-123-loaded SH-OGC demonstrated effective cellular accumulation via caveola-mediated endocytosis along with the inhibition of P-gp efflux. Furthermore, Caco-2 transport studies demonstrated that the mechanistic basis of SH-OGC efficacy was attributed to P-gp inhibition, enhanced permeability of tight junctions and clathrin-mediated transcytosis across the endothelium. In addition, SH-OGC exhibited increased intestinal retention through thiol-mediated mucoadhesion compared with OGC according to results of mucoadhesion evaluation on freshly excised rat intestine. In summary, SH-OGC micelles may present as a promising delivery vehicle for enhancing the oral bioavailability of P-gp substrates. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Activity coefficients at infinite dilution of organic solutes in the ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate using gas-liquid chromatography at T = (313.15, 323.15, and 333.15) K

    International Nuclear Information System (INIS)

    Olivier, Eugene; Letcher, Trevor M.; Naidoo, Paramespri; Ramjugernath, Deresh

    2010-01-01

    Activity coefficients at infinite dilution were determined for 24 solutes: n-alkanes, alk-1-enes, alk-1-ynes, cycloalkanes, alkylbenzenes and alcohols in the ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate, [OMIM][PF 6 ], by gas-liquid chromatography at three different temperatures T = (313.15, 323.15, and 333.15) K. The partial molar excess enthalpy values at infinite dilution were calculated from the experimental data over the same temperature range. Capacities and selectivities at infinite dilution for the systems hexane/benzene and methanol/benzene were determined from the experimental data and compared to the literature values for other ionic liquids, as well as for industrial molecular solvents. The influence of the cation and anion of the ionic liquid on the activity coefficient is discussed, as well as the usefulness of [OMIM][PF 6 ] in separating organic liquids.

  10. Deuterium kinetic isotope effects in the 1,4-dimethylenecyclohexane boat cope rearrangement

    International Nuclear Information System (INIS)

    Gajewski, J.J.; Jimenez, J.L.

    1986-01-01

    In order to examine the extent of bond making in the boat-like 3,3-sigmatropic shift transition states, trans-2,3-dimethyl-1,4-dimethylenecyclohexane (T) and its exomethylene tetradeuteria derivative (TXD) were prepared. The 3,3-shift of TXD at 305 0 C results in interconversion of starting material, 5,5,6,6-tetradeuterio-trans-2,3-dimethyl-1,4-dimethylene-cyclohexane (TND), and 2,2,3,3-tetradeuterio-anti-1,4-diethylidenecyclohexane (AD). A kinetic analysis of the first-order rate equations for the three-component system in both protio and deuterio species by numerical integration of the data and simplex minimization of the rate constants with symmetry and the assumption of no equilibrium or kinetic isotope effect on the TND-AD reaction gives a bond making kinetic isotope effect of 1/1.04 (0.04). The equilibrium isotope effects observed are 1/1.16 (0.04) so that the extent of bond formation in this boat-like bicyclo[2.2.2]octyl transition state is roughly 25%, a value to be compared with ca. 67% in chair-like acyclic 3,3-shift transition states. This rules out significant intervention of a bicyclo[2.2.2]octane-1,4-diyl intermediate or transition state. 30 references, 6 figures, 4 tables

  11. Crystal structure of 2-cyano-1-methylpyridinium bromide

    Directory of Open Access Journals (Sweden)

    Vu D. Nguyen

    2015-11-01

    Full Text Available In the title molecular salt, C7H7N2+·Br−, all the non-H atoms lie on crystallographic mirror planes. The packing consists of (010 cation–anion layers, with the cations forming dimeric units via very weak pairwise C—H...N interactions. Weak C—H...Br interactions link the cations to the anions.

  12. The Octyl Ester of Ginsenoside Rh2 Induces Lysosomal Membrane Permeabilization via Bax Translocation

    Directory of Open Access Journals (Sweden)

    Fang Chen

    2016-04-01

    Full Text Available Ginsenoside Rh2 is a potential pharmacologically active metabolite of ginseng. Previously, we have reported that an octyl ester derivative of ginsenoside Rh2 (Rh2-O, has been confirmed to possess higher bioavailability and anticancer effect than Rh2 in vitro. In order to better assess the possibility that Rh2-O could be used as an anticancer compound, the underlying mechanism was investigated in this study. The present results revealed that lysosomal destabilization was involved in the early stage of cell apoptosis in HepG2 cells induced by Rh2-O. Rh2-O could induce an early lysosomal membrane permeabilization with the release of lysosomal protease cathepsins to the cytosol in HepG2 cells. The Cat B inhibitor (leu and Cat D inhibitor (pepA inhibited Rh2-O-induced HepG2 apoptosis as well as tBid production and Δφm depolarization, indicating that lysosomal permeabilization occurred upstream of mitochondrial dysfunction. In addition, Rh2-O induced a significant increase in the protein levels of DRAM1 and Bax (p < 0.05 in lysosomes of HepG2 cells. Knockdown of Bax partially inhibited Rh2-O-induced Cat D release from lysosomes. Thus it was concluded that Rh2-O induced apoptosis of HepG2 cells through activation of the lysosomal-mitochondrial apoptotic pathway involving the translocation of Bax to the lysosome.

  13. A comparison of 2-octyl cyanoacrylate with nylon for wound closure of knee arthroscopy portals.

    Science.gov (United States)

    Imbuldeniya, A M; Rashid, A; Murphy, J P

    2014-09-01

    To compare the cosmetic results, complications and patient satisfaction of 2-octyl cyanoacrylate (Dermabond, Ethicon Inc. Somerville, NJ, USA), a liquid bonding agent, with 3-0 nylon sutures (Ethilon, Ethicon Inc) skin closure in two groups of patients undergoing elective knee arthroscopy at 6 weeks. The retrospective clinical audit recruited patients undergoing knee surgery for the first time between October 2010 and August 2011. The patients were either treated with the liquid bonding agent or nylon sutures. The patients in the bonding agent group were allowed to shower as normal on postoperative day one, while patients in the suture group kept their wounds dry for 2 weeks. Between the two groups (40 patients per group) there was no difference in the cosmetic outcome (p=0.285), patient satisfaction (p=0.29), pain scores (p=0.44) or wound complication rate (pfinance was received for this study, nor any input from other sources.

  14. Phase equilibrium properties of binary aqueous solutions containing ethanediamine, 1,2-diaminopropane, 1,3-diaminopropane, or 1,4-diaminobutane at several temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Nouria Chiali-Baba [LATA2M, Laboratoire de Thermodynamique Appliquee et Modelisation Moleculaire, University AbouBekr Belkaid of Tlemcen, P.O. Box 119, Tlemcen 13000 (Algeria); Negadi, Latifa, E-mail: l_negadi@mail.univ-tlemcen.d [LATA2M, Laboratoire de Thermodynamique Appliquee et Modelisation Moleculaire, University AbouBekr Belkaid of Tlemcen, P.O. Box 119, Tlemcen 13000 (Algeria); Mokbel, Ilham; Jose, Jacques [LSA, Laboratoire des Sciences Analytiques, CNRS-UMR 5180, Universite Claude Bernard - Lyon I. 43, Bd du 11 Novembre 1918, Villeurbanne Cedex 69622 (France)

    2011-05-15

    Research highlights: Vapour pressures of ethanediamine (EDA), 1,2-diaminopropane, 1,3-diaminopropane (1,3-DAP), or 1,4-diaminobutane (1,4-DAB) aqueous solutions are reported between (293 and 363) K. The two first mixtures show negative azeotropic behaviour. The aqueous solutions of EDA, 1,2-DAP, or 1,3-DAP exhibit negative G{sup E} whereas the one containing 1,4-DAB shows either negative G{sup E} or sinusoidal shape for G{sup E}. - Abstract: The vapour pressures of {l_brace}ethanediamine (EDA) + water{r_brace}, {l_brace}1,2-diaminopropane (1,2-DAP) + water{r_brace}, {l_brace}1,3-diaminopropane (1,3-DAP) + water{r_brace} or {l_brace}1,4-diaminobutane (1,4-DAB) + water{r_brace} binary mixtures, and of pure EDA, 1,2-DAP, 1,3-DAP, 1,4-DAB, and water components were measured by means of two static devices at temperatures between (293 and 363) K. The data were correlated with the Antoine equation. From these data, the excess Gibbs function (G{sup E}) was calculated for several constant temperatures and fitted to a fourth-order Redlich-Kister equation using the Barker's method. The {l_brace}ethanediamine (EDA) + water{r_brace}, and {l_brace}1,2-diaminopropane (1,2-DAP) + water{r_brace} binary systems show negative azeotropic behaviour. The aqueous solutions of EDA, 1,2-DAP, or 1,3-DAP exhibit negative deviations in G{sup E} for all investigated temperatures over the whole composition range whereas the (1,4-DAB + water) binary mixture shows negative G{sup E} for temperatures (293.15 < T/K < 353.15) and a sinusoidal shape for G{sup E} at T = 363.15 K.

  15. 5-Bromo-1-octylindoline-2,3-dione

    Directory of Open Access Journals (Sweden)

    Yassine Kharbach

    2016-03-01

    Full Text Available The title compound, C16H20BrNO2, crystallizes with two molecules in the asymmetric unit. The indoline ring system and the two ketone O atoms are nearly coplanar, with the largest deviations from the mean plane being 0.077 (2 and 0.055 (2 Å in the two molecules. In each molecule, the mean plane through the octyl chain is nearly perpendicular to the mean plane of the indoline ring system, as indicated by the dihedral angles between them of 86.6 (1 and 76.1 (1°. In the crystal, molecules are linked by week C—H...O hydrogen bonds, forming a three-dimensional network.

  16. Thermodynamic behavior of binary mixtures CnMpyNTf2 ionic liquids with primary and secondary alcohols

    International Nuclear Information System (INIS)

    Calvar, N.; Gómez, E.; Domínguez, Á.; Macedo, E.A.

    2012-01-01

    Highlights: ► Osmotic coefficients of alcohols with C n MpyNTf 2 (n = 2, 3, 4) are determined. ► Experimental data were correlated with Extended Pitzer model of Archer and MNRTL. ► Mean molal activity coefficients and excess Gibbs free energies were calculated. ► The results have been interpreted in terms of interactions. - Abstract: In this paper, the osmotic and activity coefficients and vapor pressures of the binary mixtures containing the ionic liquids 1-ethyl-3-methylpyridinium bis(trifluoromethylsulfonyl)imide, C 2 MpyNTf 2 , and 1-methyl-3-propylpyridinium bis(trifluoromethylsulfonyl)imide, C 3 MpyNTf 2 , with 1-propanol, or 2-propanol and the ionic liquid 1-butyl-3-methylpyridinium bis(trifluoromethylsulfonyl)imide, C 4 MpyNTf 2 , with 1-propanol or 2-propanol or 1-butanol or 2-butanol were determined at T = 323.15 K using the vapor pressure osmometry technique. The influence of the structure of the alcohol and of the ionic liquid on both coefficients and vapor pressures is discussed and a comparison with literature data on binary mixtures containing ionic liquids with different cations and anion is also performed. Besides, the results have been interpreted in terms of solute–solvent and ion–ion interactions. The experimental osmotic coefficients were correlated using the Extended Pitzer model of Archer and the Modified Non-Random Two Liquids model obtaining standard deviations lower than 0.059 and 0.102 respectively, and the mean molal activity coefficients and the excess Gibbs free energy for the studied mixtures were calculated.

  17. Structural characterization and DFT study of a new optical crystal: 2-amino-3-methylpyridinium-3,5-dinitrobenzoate

    Science.gov (United States)

    Sathya, K.; Dhamodharan, P.; Dhandapani, M.

    2018-05-01

    A new proton transfer complex was synthesized by the reaction between 2-amino-3-methyl pyridine with 3,5-dinitro benzoic acid in methanol solvent at room temperature. Chemical composition and stoichiometry of the synthesized complex 2-amino-3-methylpyridinium 3,5-dinitrobenzoate (AMPDB) were verified by CHN analysis. The AMPDB crystals were subjected to FT-IR spectral analysis to confirm the functional groups in the compound. UV-Vis-NIR spectral studies revealed that the AMPDB has a large optical transparency window. Single crystal XRD analysis reveals that AMPDB belongs to a monoclinic system with P21/c space group. NMR spectroscopic data indicate the exact carbon skeleton and hydrogen environment in the molecular structure of AMPDB. The thermal stability of the compound was investigated by thermogravimetry (TG). Computational studies such as optimisation of molecular geometry, natural bond analysis (NBO), Mulliken population analysis and HOMO-LUMO analysis were performed using Gaussian 09 software by B3LYP method at 6-311 G(d p) basis set. The first order hyperpolarizability (β) value is 37 times greater than that of urea. The optical nonlinearities of AMPDB have been investigated by Z-scan technique with He-Ne laser radiation of wavelength 632.8 nm. Hirshfeld analysis indicate O⋯H/H⋯O interactions are the superior interactions confirming intensive hydrogen bond net work.

  18. Volumetric and surface properties of pure ionic liquid n-octyl-pyridinium nitrate and its binary mixture with alcohol

    International Nuclear Information System (INIS)

    Jiang Haichao; Wang Jianying; Zhao Fengyun; Qi Guodi; Hu Yongqi

    2012-01-01

    Highlights: ► Density and surface tension of [Ocpy][NO 3 ] were measured. ► Thermal expansion coefficient, molecular volume, and standard entropies were obtained. ► The critical temperature and enthalpy of vaporization were discussed. ► Density and surface tension were measured for (ionic liquid + alcohols) mixtures. ► Excess molar volumes and surface tension deviations were fitted to Redlich–Kister equation. - Abstract: The density and surface tension for pure ionic liquid N-octyl-pyridinium nitrate were measured from (293.15 to 328.15) K. The coefficient of thermal expansion, molecular volume, standard entropies, and lattice energy were calculated from the experimental density values. The critical temperature, surface entropy, surface enthalpy, and enthalpy of vaporization were also studied from the experimental surface tension results. Density and surface tension were also determined for binary mixtures of (N-octyl-pyridinium nitrate + alcohol) (methanol, ethanol, and 1-butanol) systems over the whole composition range at 298.15 K and atmospheric pressure. Excess molar volumes and surface tension deviations for the binary systems have been calculated and were fitted to a Redlich–Kister equation to determine the fitting parameters and the root mean square deviations. The partial molar volume, excess partial molar volume, and apparent molar volume of the component IL and alcohol in the binary mixtures were also discussed.

  19. Thermodynamic properties of binary mixtures combining two pyridinium-based ionic liquids and two alkanols

    International Nuclear Information System (INIS)

    García-Mardones, Mónica; Barrós, Alba; Bandrés, Isabel; Artigas, Héctor; Lafuente, Carlos

    2012-01-01

    Highlights: ► Thermodynamic properties of an ionic liquid and an alkanol have been reported. ► The ionic liquids studied were 1-butyl-3 (or 4)-methylpyridinium tetrafluoroborate. ► The alkanols were methanol and ethanol. ► From measured data excess properties have been obtained and correlated. - Abstract: Densities and speeds of sound have been determined for the binary mixtures containing an ionic liquid (1-butyl-3-methylpyridinium tetrafluoroborate or 1-butyl-4-methylpyridinium tetrafluoroborate) and an alkanol (methanol or ethanol) over the temperature range (293.15 to 323.15) K. Excess volumes and excess isentropic compressibilities have been calculated from density and speed of sound data and correlated. All the mixtures show negative values for these excess properties. Furthermore, the isothermal (vapour + liquid) equilibrium has been measured at T = (303.15 and 323.15) K, and the corresponding activity coefficients and excess Gibbs functions have been obtained. In this case, positive excess Gibbs functions have been found. We have carried out an exhaustive interpretation of the experimental results in terms of structural and energetic effects taking also into account the thermodynamic information of pure compounds. Finally, in order to study the influence of both, the presence and the position of methyl group in the cation, we have compared the results of these systems with those obtained for the mixtures formed by 1-butylpyridinium tetrafluoroborate and methanol or ethanol.

  20. Desorption of Lipases Immobilized on Octyl-Agarose Beads and Coated with Ionic Polymers after Thermal Inactivation. Stronger Adsorption of Polymers/Unfolded Protein Composites

    Directory of Open Access Journals (Sweden)

    Jose J. Virgen-Ortíz

    2017-01-01

    Full Text Available Lipases from Candida antarctica (isoform B and Rhizomucor miehei (CALB and RML have been immobilized on octyl-agarose (OC and further coated with polyethylenimine (PEI and dextran sulfate (DS. The enzymes just immobilized on OC supports could be easily released from the support using 2% SDS at pH 7, both intact or after thermal inactivation (in fact, after inactivation most enzyme molecules were already desorbed. The coating with PEI and DS greatly reduced the enzyme release during thermal inactivation and improved enzyme stability. However, using OC-CALB/RML-PEI-DS, the full release of the immobilized enzyme to reuse the support required more drastic conditions: a pH value of 3, a buffer concentration over 2 M, and temperatures above 45 °C. However, even these conditions were not able to fully release the thermally inactivated enzyme molecules from the support, being necessary to increase the buffer concentration to 4 M sodium phosphate and decrease the pH to 2.5. The formation of unfolded protein/polymers composites seems to be responsible for this strong interaction between the octyl and some anionic groups of OC supports. The support could be reused five cycles using these conditions with similar loading capacity of the support and stability of the immobilized enzyme.

  1. (1-Butyl-4-methyl-pyridinium)[Cu(SCN)2]: a coordination polymer and ionic liquid.

    Science.gov (United States)

    Spielberg, Eike T; Edengeiser, Eugen; Mallick, Bert; Havenith, Martina; Mudring, Anja-Verena

    2014-04-25

    The compound (C4C1py)[Cu(SCN)2], (C4C1py = 1-Butyl-4-methyl-pyridinium), which can be obtained from CuSCN and the ionic liquid (C4C1py)(SCN), turns out to be a new organic-inorganic hybrid material as it qualifies both, as a coordination polymer and an ionic liquid. It features linked [Cu(SCN)2](-) units, in which the thiocyanates bridge the copper ions in a μ1,3-fashion. The resulting one-dimensional chains run along the a axis, separated by the C4C1py counterions. Powder X-ray diffraction not only confirms the single-crystal X-ray structure solution but proves the reformation of the coordination polymer from an isotropic melt. However, the materials shows a complex thermal behavior often encountered for ionic liquids such as a strong tendency to form a supercooled melt. At a relatively high cooling rate, glass formation is observed. When heating this melt in differential scanning calorimetry (DSC) and temperature-dependent polarizing optical microscopy (POM), investigations reveal the existence of a less thermodynamically stable crystalline polymorph. Raman measurements conducted at 10 and 100 °C point towards the formation of polyanionic chain fragments in the melt. Solid-state UV/Vis spectroscopy shows a broad absorption band around 18,870 cm(-1) (530 nm) and another strong one below 20,000 cm(-1) (<500 nm). The latter is attributed to the d(Cu(I))→π*(SCN)-MLCT (metal-to-ligand charge transfer) transition within the coordination polymer yielding an energy gap of 2.4 eV. At room temperature and upon irradiation with UV light, the material shows a weak fluorescence band at 15,870 cm(-1) (630 nm) with a quantum efficiency of 0.90(2) % and a lifetime of 131(2) ns. Upon lowering the temperature, the luminescence intensity strongly increases. Simultaneously, the band around 450 nm in the excitation spectrum decreases. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. 4-[2-(4-cyanophenyl)ethenyl]-N-methylpyridinium tetraphenylborate.

    Science.gov (United States)

    Jin, Dan; Zhang, De Chun

    2005-11-01

    In the title compound, C(15)H(13)N(2)(+).C(24)H(20)B(-), the pyridyl ring of the cation makes a dihedral angle of 1.6 degrees with the benzene ring. Each is rotated in the same direction with respect to the central -C-CH=CH-C- linkage, by 3.8 and 5.3 degrees, respectively. The anions have a slightly distorted tetrahedral geometry. Molecular packing analysis was carried out using the packing energy portioning scheme in the program OPEC. Around each anion in the crystal structure there are eight anions, which interact with the central anion through C-H...pi interactions. The cations are hydrogen bonded in a head-to-tail fashion, forming chains along [101].

  3. Friction Blisters on the Hands Treated Successfully Using 2-Octyl Cyanoacrylate: A Case Report.

    Science.gov (United States)

    Gearhart, Peter A; Gaspar, Michael P; Jacoby, Sidney M

    Friction blisters on the hand are challenging to treat as conventional dressings are prone to saturation, contamination, and loosening with active hand use and other mechanical stresses. Alternative methods and materials for dressing hand blisters warrant exploration. A 48-year-old male surgeon presented with friction blisters over his bilateral thumbs. The patient complained of significant difficulty in keeping his dressings clean and dry, significant pain with hand hygiene, and functional limitations at work. The patient's blisters were dressed with 2-octyl cyanoacrylate (Dermabond; Ethicon US LLC, Somerville, New Jersey), applied directly onto the wound bed. The patient was able to perform his normal duties immediately, without the need for additional intervention. Six days postapplication, the Dermabond sloughed off, revealing an epithelialized surface. Dermabond is a promising agent for dressing unroofed blisters of the hand, as it provides a barrier to moisture and contamination, while allowing the wound to epithelialize, without functional cost.

  4. Hepatic Proteomic Responses in Marine Medaka ( Oryzias melastigma ) Chronically Exposed to Antifouling Compound Butenolide [5-octylfuran-2(5H)-one] or 4,5-Dichloro-2- N -Octyl-4-Isothiazolin-3-One (DCOIT)

    KAUST Repository

    Chen, Lianguo

    2015-02-03

    The pollution of antifoulant SeaNine 211, with 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) as active ingredient, in coastal environment raises concerns on its adverse effects, including endocrine disruption and impairment of reproductive function in marine organisms. In the present study, we investigated the hepatic protein expression profiles of both male and female marine medaka (Oryzias melastigma) exposed to low concentrations of DCOIT at 2.55 mu g/L (0.009 mu M) or butenolide, a promising antifouling agent, at 2.31 mu g/L (0.012 mu M) for 28 days. The results showed that proteins involved in phase I (CYP450 enzyme) metabolism, phase II (UDPGT and GST) conjugation as well as mobilization of retinoid storage, an effective nonenzymatic antioxidant, were consistently up-regulated, possibly facilitating the accelerated detoxification of butenolide. Increased synthesis of bile acid would promote the immediate excretion of butenolide metabolites. Activation of fatty acid beta-oxidation and ATP synthesis were consistent with elevated energy consumption for butenolide degradation and excretion. However, DCOIT did not significantly affect the detoxification system of male medaka, but induced a marked increase of vitellogenin (VTG) by 2.3-fold in the liver of male medaka, suggesting that there is estrogenic activity of DCOIT in endocrine disruption. Overall, this study identified the molecular mechanisms and provided sensitive biomarkers characteristic of butenolide and DCOIT in the liver of marine medaka. The low concentrations of butenolide and DCOIT used in the exposure regimes highlight the needs for systematic evaluation of their environmental risk. In addition, the potent estrogenic activity of DCOIT should be considered in the continued applications of SeaNine 211.

  5. Synthesis and physical-chemical properties of 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R-2,4-dihydro-3H-1,2,4-triazoles

    Directory of Open Access Journals (Sweden)

    T. M. Kaplaushenko

    2016-06-01

    Full Text Available The major social and economic problem of pharmaceutical industry is the search for biologically active substances, which may become the basis of new drugs, competitive with expensive imported drugs. Analysis of literature shows that in recent decades the attention is paid to researches of heterocyclic systems as potential biologically active agents of both domestic and foreign scientists. Particular interest in this regard cause 3-thio derivatives of 1,2,4-triazoles. Despite high number of publications relating to synthesis and biological properties of 1,2,4-triazole derivatives, the structure and physical-chemical properties of these compounds are studied insufficiently. In this regard, the study of synthetic, physical-chemical and biological properties of 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R1-2,4-dihydro-3H-1,2,4-triazoles in our point of view is a new, theoretically and practically significant direction. Purpose - targeted synthesis of new low-toxic and highly effective compounds with potential pharmacological activity in a series of 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R-2,4-dihydro-3H-1,2,4-triazoles and the study of physical and chemical properties of the synthesized compounds. Materials and methods. As starting compounds 5-(quinoline-2-il- 2-hydroxyquinoline-4-yl-4-R1-3-thio-1,2,4-triazoles have been used. Through further cooperation with halogen alkanes (ethyl bromide, propyl bromide, amyl bromide, octyl bromide, nonyl bromide, decyl bromide, cyclohexyl chloride, benzyl chloride 3-alkylthio-5-(quinoline-2-yl, 2-hydroxyquinoline-4-yl-4-R1-2,4-dyhidro-3H-1,2,4-triazoles have been obtained. Results. 15 New compounds have been received as a result of synthetic transformations, the structure of synthesized compounds has been confirmed by modern complex of physical and chemical methods of analysis (IR-spectrophotometry, 1H NMR-spectroscopy, elemental analysis, and their individuality has been proved by

  6. Efficiency of n-octyl-acetate, 2-heptanone and citronellal in repelling bees from basil (Ocimum sellowii - Labiatae

    Directory of Open Access Journals (Sweden)

    Darclet Teresinha Malerbo-Souza

    2004-03-01

    seguida, acompanhando a curva da temperatura ambiente registrada nos dias do experimento. As abelhas africanizadas demoraram de 1 a 3 segundos em cada flor. A freqüência das abelhas africanizadas não diminuiu com a aplicação dos produtos n.octyl.acetato, citronellal e 2.heptanona, usados como repelentes, nas concentrações 2,5, 5,0, 7,5 e 10,0%, diluídos apenas em água. Entretanto, quando os produtos (20% foram diluídos em água (75% e glicerina (5%, foram efetivos em repelir essas abelhas das flores de manjericão, por um período de 20 minutos.

  7. Photolysis study of octyl p-methoxycinnamate loaded microemulsion by molecular fluorescence and chemometric approach

    Science.gov (United States)

    Nascimento, Danielle Silva; Insausti, Matías; Band, Beatriz Susana Fernández; Grünhut, Marcos

    2018-02-01

    Octyl p-methoxycinnamate (OMC) is one of the most widely used sunscreen agents. However, the efficiency of OMC as UV filter over time is affected due to the formation of the cis-isomer which presents a markedly lower extinction coefficient (εcis = 12,600 L mol- 1 cm- 1 at 291 nm) than the original trans-isomer (εtrans = 24,000 L mol- 1 cm- 1 at 310 nm). In this work, a novel carrier for OMC based on an oil-in-water microemulsion is proposed in order to improve the photostability of this sunscreen. The formulation was composed of 29.2% (w/w) of a 3:1 mixture of ethanol (co-surfactant) and decaethylene glycol mono-dodecyl ether (surfactant), 1.5% (w/w) of oleic acid (oil phase) and 69.2% (w/w) of water. This microemulsion was prepared in a simple way, under moderate stirring at 25 °C and using acceptable, biocompatible and accessible materials for topical use. OMC was incorporated in the vehicle at a final concentration of 5.0% (w/w), taking into account the maximum permitted levels established by international norms. Then, a photolysis study of the loaded formulation was performed using a continuous flow system. The direct photolysis was monitored over time by molecular fluorescence. The recorded spectra data between 370 y 490 nm were analyzed by multivariate curve resolution-alternating least squares algorithm. The kinetic rate constants corresponding to the photolysis of the trans-OMC were calculated from the concentration profiles, resulting in 0.0049 s- 1 for the trans-OMC loaded microemulsion and 0.0131 s- 1 for the trans-OMC in aqueous media. These results demonstrate a higher photostability of the trans-OMC when loaded in the proposed vehicle with respect to the free trans-OMC in aqueous media.

  8. Rapid and selective derivatizatin method for the nitrogen-sensitive detection of carboxylic acids in biological fluids prior to gas chromatographic analysis

    NARCIS (Netherlands)

    Lingeman, H.; Haan, H.B.P.; Hulshoff, A.

    1984-01-01

    A rapid and selective derivatization procedure is described for the pre-column labelling of carboxylic acids with a nitrogen-containing label. The carboxylic acid function is activated with 2-bromo-1-methylpyridinium iodide and the activated carboxylic acid function reacts with a primary or a

  9. Separation of Cu, In, Fe and Sn from nuclear grade thorium by tri-n-octyl amine-5 M HCI and their determination by atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Moraes, S. de; Cipriani, M.; Abrao, A.

    1976-01-01

    The results of solvent extraction separation of a group of metal traces in high pure thorium with the aid of tri-n-octyl amine-benzene from ThCL 4 HCI are summarized. ThCl 4 HCI-KI solutions Cu,In,Fe and Sn are extracted together and determined by atomic absoprtion spectrophotometry, burning directly the organic phase. The behavior of Cu,In,Fe and Sn toward direct burn of the organic phase using hydrogen-air mixture was studied, and an absorption enhancement was observed. The procedure is being used ot perform the quality control of nuclear grade thorium and its compounds. The calibration curves have provided precisions in the range 1 to 10% in analysis of thorium

  10. The influence of tri-n-octyl phosphine oxide and extraction stage on purification of Thorium concentrate

    International Nuclear Information System (INIS)

    M-V-Purwani; Moch-Setyadji

    2015-01-01

    The extraction of thorium oxalate concentrate as processing product of monazite using Tri Octyl Phosphine Oxide (TOPO) has been done. The most impurities contained in thorium oxalate concentrate are Ce (cerium) and La (lanthanum). The purpose of this study is to purify Th by separating Ce and La using extraction process. The extraction is done by batch and multistage. The solution of feed or water phase is 10 grams of Th oxalate concentrate dissolved in 10.08 M HNO 3 so that the volume becomes 100 mL and the organic phase is TOPO in kerosene. Stripping in each stage conducted three times, first stripping use water, second stripping use 5 % oxalic acid and the third stripping use water. Extraction time at every stage is 15 minutes and stripping time at every stage is 5 minutes with ratio of aqueous phase to organic phase = 1 : 1 . The parameters were studied % TOPO - kerosene and number of extraction stage. The optimum usage of TOPO in kerosene is 5 %. On extraction I obtained Ce concentrate and on extraction II and III obtained Th concentrates. The extraction II efficiency of Th is 39.76 % and extraction III efficiency of Th is 26.33 % . Coefficient of distribution (Kd) of Th in stage II is 0.7587 and Kd of Th in stage III is 1.0096. Total extraction efficiency of Th is 80.08 %, total extraction efficiency of Ce is 56.12 %, and total extraction efficiency of La is 1.54 %. The separation factor of Th – Ce in extraction I is 1.00 and separation factor of Th – La in extraction I is 92.0, separation factor of Th – Ce in extraction II is 250.24, and separation factor of Th – La in extraction II is ∞. Separation factor of Th – Ce in extraction III is 124.22 and separation factor of Th – La in extraction III is ∞. Total separation factor of Th – Ce is 1.4270 and total separation factor of Th – La is 4.0459. The content of Th oxalate in stripping product from the extraction II is 97.06 % and in stripping product from the extraction III is 98

  11. Separation of Cu, In, Fe and Sn from nuclear grade thorium by tri-n-octyl amine--5 M HCI and their determination by atomic absorption spectrophotometry

    Energy Technology Data Exchange (ETDEWEB)

    de Moraes, S; Cipriani, M; Abrao, A

    1976-03-01

    The results of solvent extraction separation of a group of metal traces in high pure thorium with the aid of tri-n-octyl amine-benzene from ThCl/sub 4/HCl are summarized. ThCl/sub 4/HCl-KI solutions of Cu, In, Fe and Sn are extracted together and determined by atomic absoprtion spectrophotometry and burning directly the organic phase. The behavior of Cu, In, Fe and Sn toward direct burn of the organic phase using hydrogen-air mixture was studied, and an absorption enhancement was observed. The procedure is being used to perform the quality control of nuclear grade thorium and its compounds. The calibration curves have provided precisions in the range 1 to 10% in analysis of thorium.

  12. 21 CFR 522.1862 - Sterile pralidoxime chloride.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Sterile pralidoxime chloride. 522.1862 Section 522....1862 Sterile pralidoxime chloride. (a) Chemical name. 2-Formyl-1-methylpyridinium chloride oxime. (b) Specifications. Sterile pralidoxime chloride is packaged in vials. Each vial contains 1 gram of sterile...

  13. Structure and Stability of the Spinach Aquaporin SoPIP2;1 in Detergent Micelles and Lipid Membranes

    DEFF Research Database (Denmark)

    Plasencia, Ines; Survery, Sabeen; Ibragimova, Sania

    2011-01-01

    Background: SoPIP2;1 constitutes one of the major integral proteins in spinach leaf plasma membranes and belongs to the aquaporin family. SoPIP2;1 is a highly permeable and selective water channel that has been successfully overexpressed and purified with high yields. In order to optimize...... reconstitution of the purified protein into biomimetic systems, we have here for the first time characterized the structural stability of SoPIP2;1. Methodology/Principal Finding: We have characterized the protein structural stability after purification and after reconstitution into detergent micelles...... and proteoliposomes using circular dichroism and fluorescence spectroscopy techniques. The structure of SoPIP2;1 was analyzed either with the protein solubilized with octyl-beta-D-glucopyranoside (OG) or reconstituted into lipid membranes formed by E. coli lipids, diphytanoylphosphatidylcholine (DPh...

  14. Resolution of D- and L-glucoses by chiral N-octyl-beta-D-glycoside-Cu(II) complex adsorbed at the gas/liquid interface of small bubbles

    NARCIS (Netherlands)

    Sakai, M.; Miyazawa, K.; Jitsumatsu, H.; Kamio, K.; Mitsuiki, S.; Toh, N.; Sugihara, G.; Norde, W.

    2010-01-01

    A new technique of the jet drop method (JDM) was applied to a chiral molecular discrimination of optically active D- or L-glucose (guest) by chiral N-octyl-beta-D-glycoside (O beta DG)-Cu(II) complex (host) at the gas/liquid interface of small bubbles. The discrimination of glucoses as the guests is

  15. Spatial analysis of 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (Sea-Nine 211) concentrations and probabilistic risk to marine organisms in Hiroshima Bay, Japan

    International Nuclear Information System (INIS)

    Mochida, Kazuhiko; Hano, Takeshi; Onduka, Toshimitsu; Ichihashi, Hideki; Amano, Haruna; Ito, Mana; Ito, Katsutoshi; Tanaka, Hiroyuki; Fujii, Kazunori

    2015-01-01

    We analyzed the spatial distribution of an antifouling biocide, 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (Sea-Nine 211) in the surface water and sediments of Hiroshima Bay, Japan to determine the extent of contamination by this biocide. A quantitative estimate of the environmental concentration distribution (ECD) and species sensitivity distributions (SSDs) for marine organisms were derived by using a Bayesian statistical model to carry out a probabilistic ecological risk analysis, such as calculation of the expected potentially affected fraction (EPAF). The spatial distribution analysis supported the notion that Sea-Nine 211 is used mainly for treatment of ship hulls in Japan. The calculated EPAF suggests that approximately up to a maximum of 0.45% of marine species are influenced by the toxicity of Sea-Nine 211 in Hiroshima Bay. In addition, estimation of the ecological risk with a conventional risk quotient method indicated that the risk was a cause for concern in Hiroshima Bay. - Highlights: • Spatial distribution analysis exhibits the dynamics of Sea-Nine 211 in Hiroshima Bay. • Probabilistic ecological risk of the biocide was estimated with a Bayesian approach. • Approximately up to 0.45% of marine species were possibly influenced by the toxicity. • The risk analysis concludes that Sea-Nine 211 should be a priority for further work. - Spatial distribution of an antifouling biocide and quantification of its ecological risk were elucidated

  16. Binding-Induced Fluorescence of Serotonin Transporter Ligands

    DEFF Research Database (Denmark)

    Wilson, James; Ladefoged, Lucy Kate; Babinchak, Michael

    2014-01-01

    The binding-induced fluorescence of 4-(4-(dimethylamino)-phenyl)-1-methylpyridinium (APP(+)) and two new serotonin transporter (SERT)-binding fluorescent analogues, 1-butyl-4-[4-(1-dimethylamino)phenyl]-pyridinium bromide (BPP(+)) and 1-methyl-4-[4-(1-piperidinyl)phenyl]-pyridinium (PPP(+)), has...

  17. The Analysis of Silver Nanoparticles After the Manipulation of Synthesis Parameters and with the Addition of Potassium 2-(9-Carboxy-1-Octylnonylsulfanyl)-Malonate

    International Nuclear Information System (INIS)

    Chin, S.Y.; Hakam, M.A.O.; Goh, S.C.; Yarmo, M.A.

    2011-01-01

    This research aimed to synthesize and characterize silver nanoparticles by manipulating the parameters involved in stabilizing the particles. The silver nanoparticles in this research were synthesized by reduction process of silver nitrate (AgNO 3 ) with sodium borohydrate (NaBH 4 ) as the reducing agent. The addition of potassium 2- (9-carboxy-1-octylnonylsulfanyl)-malonate into silver nanoparticles solution functioned as a stabilizing agent. The parameters involved in this research were the effect of time towards stability of silver nanoparticles, the effect of addition of potassium 2-(9-carboxy-1-octylnonylsulfanyl)- malonate and the pH level effect towards the synthesized silver nanoparticles. Based on the results obtained from Transmission Electron Microscopy (TEM), we have observed that the incorporation of potassium 2-(9-carboxy-1- octyl-nonanesulfonyl)-malonate as the stabilizing agent can prevent the agglomeration of silver nanoparticles within 16 days which is a breakthrough for the synthesis of silver nanoparticles by using sodium borohydride. The micrograph showed that the size of silver nanoparticles synthesized were within the range of 1.5 nm to 8.3 nm. In addition to that, Dynamic Light Scattering (DLS) technique was used in this research to measure the average size of the silver nanoparticles which stabilized with potassium 2-(9-carboxy-1-octyl-nonanesulfonyl)-malonate. X-Ray Diffraction (XRD) analysis was carried out to view the effect of manipulated pH level on crystalline silver nanoparticles structure. The XRD diffractogram showed the diffraction peaks which can be indexed to planes of face- centered cubic (fcc) of pure silver. (author)

  18. Evaluating the use of PAO (4 cSt polyalphaoelfin) oil instead of DOP (di-octyl phthalate) oil for measuring the aerosol capture of nuclear canister filters

    Energy Technology Data Exchange (ETDEWEB)

    Moore, Murray E. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2014-07-18

    This document details the distinction between using PAO (4 cSt polyalphaoelfin) oil instead of DOP (di-octyl phthalate) oil for measuring the aerosol capture of filters. This document is developed to justify the use of PAO rather than DOP for evaluating the performance of filters in the SAVY 4000 and Hagan containers. The design criteria (Anderson et al, 2012) for purchasing SAVY 4000 containers and the Safety Analysis Report for the SAVY 4000 Container Series specified that the filter must “capture greater than 99.97% of 0.45 μm mean diameter dioctyl phthalate (DOP) aerosol at the rated flow with a DOP concentration of 65±15 micrograms per liter.”This corresponds to a leakage percent of 0.03% (3.0x10-2). The density of DOP oil is 985 kg/m3 and the density of PAO oil is 819 kg/m3. ATI Test Inc measured the mass mean diameter of aerosol distributions produced by a single Laskin type III-A nozzle operating at a 20 psig air pressure as 0.563 μm for DOP oil and 0.549 μm for PAO oil. (See Appendix A.) For both types of oil in this document, the single fiber method calculated the leakage percent to be 4.4x10-5 for DOP oil and 4.7x10-5 for PAO oil. Although the percent error between these two quantities is 7.7%, these calculated leakage percent values are more than two orders of magnitude less than the criterion specified in the SAVY canister SAR. As a point of reference, the photometer used to measure the SAVY canister filter performance cannot resolve values for the leakage percent below 1.0x10-5. Additionally, over a range of particle sizes from 0.01 μm to 3.0 μm, there was less than 4.0x10-5 error between the calculated filter efficiency for the two types of oil at any particular particle size diameter. In conclusion, the difference between using DOP and PAO for testing SAVY canister filters is of inconsequential concern.

  19. Trapping molecular bromine: a one-dimensional bromobismuthate complex with Br2 as a linker.

    Science.gov (United States)

    Adonin, S A; Gorokh, I D; Abramov, P A; Plyusnin, P E; Sokolov, M N; Fedin, V P

    2016-03-07

    The reaction between solid (NMP)n{[BiBr4]}n (1) (NMP = N-methylpyridinium) and Br2, generated in situ in HBr solution, results in the formation of (NMP)3[Bi2Br9]·Br2 (2). In the structure of 2, dibromine molecules connect discrete binuclear [Bi2Br9](3-) anions into an extended network. Complex 2 is thermally stable (up to 150 °C).

  20. Silica Aerogels Doped with Ru(II) Tris 1,l0-Phenanthro1ine)-Electron Acceptor Dyads: Improving the Dynamic Range, Sensitivity and Response Time of Sol-Gel Based Oxygen Sensors

    Science.gov (United States)

    Kevebtusm Bucgikas; Rawashdeh, Abdel M.; Elder, Ian A.; Yang, Jinhua; Dass, Amala; Sotiriou-Leventis, Chariklia

    2005-01-01

    Complexes 1 and 2 were characterized in fluid and frozen solution and as dopants of silica aerogels. The intramolecular quenching efficiency of pendant 4-benzoyl-N-methylpyridinium group (4BzPy) is solvent dependent: emission is quenched completely in acetonitrile but not in alcohols. On the other hand, N-benzyl-N'-methylviologen (BzMeV) quenches the emission in all solvents completely. The differences are traced electrochemically to a stronger solvation effect by the alcohol in the case of 1. In fiozen matrices or absorbed on the surfaces of silica aerogel, both 1 and 2 are photoluminescent. The lack of quenching has been traced to the environmental rigidity. When doped aerogels are cooled to 77K, the emission shifts to the blue and its intensity increases in analogy to what is observed with Ru(II) complexes in media undergoing fluid-to-rigid transition. The photoluminescence of 1 and 2 from the aerogel is quenched by oxygen diffusing through the pores. In the presence of oxygen, aerogels doped with 1 can modulate their emission over a wider dynamic range than aerogels doped with 2, and both are more sensitive than aerogels doped with Ru(II) tris(1,l0- phenanthroline). In contrast to frozen solutions, the luminescent moieties in the bulk of aerogels kept at 77K are still accessible, leading to more sensitive platforms for oxygen sensors than other ambient temperature configurations.

  1. Long-term effects of di-octyl phthalate on the expression of immune-related genes in Tegillarca granosa

    Science.gov (United States)

    Wang, Ji; Li, Ye; Dai, Juan; Su, Xiurong; Li, Chenghua; Shen, Lingling

    2016-05-01

    Di-octyl phthalate (DOP) is widely used as a plasticizer in the plastics industry. As a result, DOP is often found in marine water ecosystems where many species are exposed to it. Our objective was to evaluate the effect of long-term (14 d) DOP exposure (2.6, 7.8, or 31.2 mg/L) on the expression of immunerelated genes in Tegillarca granosa. The expression of small heat shock protein (sHSPs) and tissue inhibitor of metalloproteinase (TIMP) were highest in clams exposed to 31.2 mg/L DOP on days 7 and 14. The relative expression of Tg-ferritin, superoxide dismutase (SOD), and metallothionein (MT) increased initially then decreased as the concentration of DOP increased. The hemoglobin of T. granosa (Tg-HbI) exhibited two distinct expression patterns at two time points. Our results suggest that the immune response of T. granosa against DOP pollution varies depending on the dose. Additionally, we identified some immune-related genes that are promising candidates for biomarkers of DOP.

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

    Directory of Open Access Journals (Sweden)

    Nadia A. Abdelriheem

    2017-02-01

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

  3. Vector coherent state representations of SO5 contains SU2 + SU2 contains U1 + U1 and SO5 contains U1 + U1

    International Nuclear Information System (INIS)

    Pan Feng

    1991-01-01

    VCS representations of SO 5 contains SU 2 + SU 2 contains U 1 + U 1 and SO 5 contains U 1 + U 1 are discussed. Reduced matrix elements for SO 5 contains SU 2 + SU 2 are derived. The multiplicity of a weight for SO 5 is determined by using the K-matrix technique

  4. X-ray Structural Investigation of Nonsymmetrically and Symmetrically Alkylated [1]Benzothieno[3,2-b]benzothiophene Derivatives in Bulk and Thin Films.

    OpenAIRE

    Gbabode , Gabin; Dohr , Michael; Niebel , Claude; Balandier , Jean-Yves; Ruzié , Christian; Négrier , Philippe; Mondieig , Denise; Geerts , Yves H; Resel , Roland; Sferrazza , Michele

    2014-01-01

    International audience; A detailed structural study of the bulk and thin film phases observed for two potential high-performance organic semiconductors has been carried out. The molecules are based on [1]benzothieno[3,2-b]benzothiophene (BTBT) as conjugated core and octyl side groups, which are anchored either symmetrically at both sides of the BTBT core (C8-BTBT-C8) or nonsymmetrically at one side only (C8-BTBT). Thin films of different thickness (8-85 nm) have been prepared by spin-coating ...

  5. Comparative safety of the antifouling compound butenolide and 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) to the marine medaka (Oryzias melastigma).

    Science.gov (United States)

    Chen, Lianguo; Ye, Rui; Xu, Ying; Gao, Zhaoming; Au, Doris W T; Qian, Pei-Yuan

    2014-04-01

    This study evaluated the potential adverse effects of butenolide, a promising antifouling compound, using the marine medaka (Oryzias melastigma), a model fish for marine ecotoxicology. The active ingredient used in the commercial antifoulant SeaNine 211, 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) was employed as the positive control. Adult marine medaka (4-month-old) were exposed to various concentrations of butenolide or DCOIT for 28 days and then depurated in clean seawater for 14 days (recovery). A suite of sensitive biomarkers, including hepatic oxidative stress, neuronal signal transmission, endocrine disruption, and reproductive function, was used to measure significant biological effects induced by the chemicals. Compared to DCOIT, chronic exposure to butenolide induced a lower extent of oxidative stress in the liver of male and female medaka. Furthermore, butenolide-exposed fish could recover faster from oxidative stress than fish exposed to DCOIT. Regarding neurotransmission, DCOIT significantly inhibited acetylcholinesterase (AChE) activity in the brain of both male and female medaka, whereas this was not significant for butenolide. In addition, plasma estradiol (E2) level was elevated and testosterone (T) level was decreased in male medaka exposed to DCOIT. This greatly imbalanced sex hormones ratio (E2/T) in exposed males, indicating that DCOIT is a potent endocrine disruptive chemical. In contrast, butenolide induced only moderate effects on sex hormone levels in exposed males, which could be gradually recovered during depuration. Moreover, the endocrine disruptive effect induced by butenolide did not affect normal development of offspring. In contrast, DCOIT-exposed fish exhibited a decrease of egg production and impaired reproductive success. Overall, the above findings demonstrated that chronic exposure to butenolide induced transient, reversible biological effect on marine medaka, while DCOIT could impair reproductive success of fish, as

  6. Comparative safety of the antifouling compound butenolide and 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) to the marine medaka (Oryzias melastigma)

    KAUST Repository

    Chen, Lianguo

    2014-04-01

    This study evaluated the potential adverse effects of butenolide, a promising antifouling compound, using the marine medaka (Oryzias melastigma), a model fish for marine ecotoxicology. The active ingredient used in the commercial antifoulant SeaNine 211, 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) was employed as the positive control. Adult marine medaka (4-month-old) were exposed to various concentrations of butenolide or DCOIT for 28 days and then depurated in clean seawater for 14 days (recovery). A suite of sensitive biomarkers, including hepatic oxidative stress, neuronal signal transmission, endocrine disruption, and reproductive function, was used to measure significant biological effects induced by the chemicals. Compared to DCOIT, chronic exposure to butenolide induced a lower extent of oxidative stress in the liver of male and female medaka. Furthermore, butenolide-exposed fish could recover faster from oxidative stress than fish exposed to DCOIT. Regarding neurotransmission, DCOIT significantly inhibited acetylcholinesterase (AChE) activity in the brain of both male and female medaka, whereas this was not significant for butenolide. In addition, plasma estradiol (E2) level was elevated and testosterone (T) level was decreased in male medaka exposed to DCOIT. This greatly imbalanced sex hormones ratio (E2/T) in exposed males, indicating that DCOIT is a potent endocrine disruptive chemical. In contrast, butenolide induced only moderate effects on sex hormone levels in exposed males, which could be gradually recovered during depuration. Moreover, the endocrine disruptive effect induced by butenolide did not affect normal development of offspring. In contrast, DCOIT-exposed fish exhibited a decrease of egg production and impaired reproductive success. Overall, the above findings demonstrated that chronic exposure to butenolide induced transient, reversible biological effect on marine medaka, while DCOIT could impair reproductive success of fish, as

  7. Preparation of nuclear pure uranium trioxide from El Atshan crude yellow cake using Tri-octyl-phosphine oxide

    Energy Technology Data Exchange (ETDEWEB)

    Hammad, A K; Serag, H M [Nuclear materials authority, (Egypt); Abdallah, A M [Faculty of science, university of mansoura, (Egypt)

    1995-10-01

    Tri n-octyl phosphine oxide (TOPO) has been investigated as a refinery extractant for crude yellow cake prepared from El Atshan ore, Eastern Desert, Egypt. Relevant factors namely: type and concentration of acid, TOPO concentration, effect of temperature, residence time and organic/ aqueous ratio have been studied and optimized. The required number of extraction and stages was determined. Further purification could be achieved for the final product by selective precipitation of uranium peroxide from the stripped solution using hydrogen peroxide followed by its calcination. Complete chemical analysis of the final product has proved its nuclear purity. 8 figs., 3 tabs.

  8. Preparation of nuclear pure uranium trioxide from El Atshan crude yellow cake using Tri-octyl-phosphine oxide

    International Nuclear Information System (INIS)

    Hammad, A.K.; Serag, H.M.; Abdallah, A.M.

    1995-01-01

    Tri n-octyl phosphine oxide (TOPO) has been investigated as a refinery extractant for crude yellow cake prepared from El Atshan ore, Eastern Desert, Egypt. Relevant factors namely: type and concentration of acid, TOPO concentration, effect of temperature, residence time and organic/ aqueous ratio have been studied and optimized. The required number of extraction and stages was determined. Further purification could be achieved for the final product by selective precipitation of uranium peroxide from the stripped solution using hydrogen peroxide followed by its calcination. Complete chemical analysis of the final product has proved its nuclear purity. 8 figs., 3 tabs

  9. Fragrance material review on 1-(2,4,4,5,5-pentamethyl-1-cyclopenten-1-yl)ethan-1-one.

    Science.gov (United States)

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

    2013-12-01

    A toxicologic and dermatologic review of 1-(2,4,4,5,5-pentamethyl-1-cyclopenten-1-yl)ethan-1-one when used as a fragrance ingredient is presented. 1-(2,4,4,5,5-Pentamethyl-1-cyclopenten-1-yl)ethan-1-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 1-(2,4,4,5,5-pentamethyl-1-cyclopenten-1-yl)ethan-1-one were evaluated then summarized and includes physical properties, acute toxicity, skin irritation, mucous membrane (eye) irritation, skin sensitization, phototoxicity, and photoallergy data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones When Used as Fragrance Ingredients (submitted for publication)) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. 1,5-Dimethyl-2-phenyl-1H-pyrazol-3(2H-one–4,4′-(propane-2,2-diylbis[1,5-dimethyl-2-phenyl-1H-pyrazol-3(2H-one] (1/1

    Directory of Open Access Journals (Sweden)

    Krzysztof Lyczko

    2013-01-01

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

  11. Synthesis and application of a macroporous silica-based polymeric octyl(phenyl)-N,N-diisobutylcarbamoylmethylphoshine oxide composite for the chromatographic separation of high level liquid waste

    International Nuclear Information System (INIS)

    Zhang, A.

    2006-01-01

    The Minor Actinides Recovery from HLW by Extraction Chromatography (MAREC) process was used mainly for the separation of minor actinides (MAs) and some specific fission products (FPs) from highly active liquid waste (HLW) by the composite CMPO/SiO 2 -P of the macroporous silica based polymeric octyl(phenyl)-N,N-diisobutylcarbamoylmethylphoshine oxide (CMPO) and others. In this study a cascade of chromatographic separation was performed on a 3.0M HNO 3 solution containing 5.0 x 10 -3 M of 13 elements, at 323 K. The cascade consisted of three columns the first and second ones were packed with CMPO/SiO 2 -P and the third with SiO 2 -P particles. The first column was employed to prepare various eluents containing saturated CMPO. The second column was used for separation into groups. The CMPO of CMPO/SiO2-P was recovered from the effluent by the third column and a CMPO-free effluent containing minor actinides was obtained. The elements contained in the simulated HLW of 3.0M HNO 3 were separated into (1) a non-adsorption group (Sr, Cs, and Ru etc.), (2) a MA-hRE (heavy rare earth)-Mo-Zr group, and (3) a lRE (light rare earth) group by eluting with 3.0M HNO 3 , 0.05M DTPA (diethylenetriaminepentaacetic acid) (pH 2.0) and HNO 3 (pH 3.5), respectively. The resultant MA-hRE-Mo-Zr mixture containing minor actinides was then separated into the groups (1) Pd-Ru, (2) MA-hRE, and (3) Mo-Zr by utilizing 3.0M HNO 3 , distilled water, and 0.05M DTPA (pH 2.0) as eluents. More than 92% of CMPO in the MA-hRE containing effluent was adsorbed by SiO 2 -P particles. The effectivity and technical feasibility of MAREC process were demonstrated. (author)

  12. Synthesis and optical properties of novel pyrido[1,2-a]benzimidazole-containing 1,3,4-oxadiazole derivatives

    International Nuclear Information System (INIS)

    Yang He; Ge Yanqing; Jia Jiong; Wang Jianwu

    2011-01-01

    A series of novel substituted 1,3,4-oxadiazole derivatives containing pyrido[1,2-a]benzimidazole moiety were synthesized and characterized using FTIR, 1 H NMR, 13 C NMR, and HRMS. An efficient tandem reaction was employed as a key step in constructing the pyrido[1,2-a]benzimidazole moiety under very mild condition. The structure of compound 4a was established by X-ray crystallography. The UV-vis absorption and fluorescence spectral characteristics of these compounds were investigated in several solvents. Compounds 4a-i display similar absorptions, with absorption peaks ranging from 330 to 339 nm in acetonitrile, while the absorption maxima of compound 4j bearing a diphenylamino group on the benzene ring is red-shifted distinctly to 377 nm due to the strong electron-donating property of its substituent and extended π-conjugated system. All these target heterocyclic compounds present blue-green emissions (461-487 nm) in dilute solutions and show high quantum yields of fluorescence (φ PL =0.65-0.99) in dichloromethane. - Research Highlights: → The first report about the unique optical properties of pyrido[1,2-a]benzimidazole heteroaromatic compounds containing 1,3,4-oxadiazole unit. → Synthesis of pyrido[1,2-a]benzimidazole moiety via a novel efficient tandem reaction. → The target heterocyclic compounds showing high quantum yields of fluorescence, with great potential for use as fluorescent pigments and in optical/electro devices.

  13. Synthesis and characterization of n-alkylamino derivatives of vitamin K3: Molecular structure of 2-propylamino-3-methyl-1,4-naphthoquinone and antibacterial activities

    Science.gov (United States)

    Chadar, Dattatray; Camilles, Maria; Patil, Rishikesh; Khan, Ayesha; Weyhermüller, Thomas; Salunke-Gawali, Sunita

    2015-04-01

    We would like to introduce eight analogues of n-alkylamino derivatives of vitamin K3 (2-methyl-1,4-naphthoquinone) viz, 2-(n-alkylamino)-3-methyl-1,4-naphthoquinone (where n-alkyl is methyl; LM-1, ethyl; LM-2, propyl; LM-3, butyl; LM-4, pentyl; LM-5, hexyl; LM-6, heptyl; LM-7, octyl; LM-8). All the above analogues have been successfully synthesized from vitamin K3 and characterized using different analytical techniques. Furthermore, in order to understand the mechanistic aspects of formation of LM-1 to LM-8 compounds, we could propose the mechanism. The FT-IR analysis of LM-1 to LM-8 indicate the presence of characteristic band of Nsbnd H group ∼3287-3364 cm-1, the variation was attributed to extensive intramolecular hydrogen bonding interaction. The molecular structure of LM-3 compound has been confirmed by single crystal X-ray diffraction analysis. LM-3 compound crystallises in triclinic space group P1. There were four independent molecules in asymmetric unit cell and their molecular interactions observed via Nsbnd H⋯O, Csbnd H⋯O and π-π stacking of quinonoid rings. Pharmacological potential of all compounds has been evaluated in terms of their antibacterial activities against Pseudomonas aeruginosa and Staphylococcus aureus. All the compounds were active against both the strains while LM-2 was found to be more effective with a minimum inhibition concentration of 0.3125 μg/mL and 0.156 μg/mL respectively.

  14. Extraction of {sup 95}(Zr, Nb) from oxalic acid solutions by means of tri-iso-octyl amine, Annex 8

    Energy Technology Data Exchange (ETDEWEB)

    Susic, M V; Maksimovic, Z B [Institute of Nuclear Sciences Boris Kidric, Laboratorija za visoku aktivnost, Vinca, Beograd (Serbia and Montenegro)

    1963-12-15

    The extractability of {sup 95}(Zr, Nb) with tri-iso-octyl amine in xylene from an oxalic acid solution has been investigated. The behaviour of uranium and other fission products has also been observed. The extraction of {sup 95}(Zr, Nb) has been studied as u function of oxalic acid and amine concentrations. Effects of the aqueous phase pH, uranium and the presence of other electrolytes have also been observed and the possibility of separating {sup 95}(Zr, Nb) from uranium and from other fission products considered (author)

  15. Ortho-substituent correlated retention of polychlorinated biphenyls on a 50% n-octyl-methylpolysiloxane stationary phase by HRGC/MSD

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, R.; Ballschmiter, K.

    1988-11-01

    Polychlorinated biphenyls (PCB) have been known as ubiquitous environmental pollutants since the late 60s. They are found partitioned between all environmental compartments according to their physico-chemical properties. Investigation of their partitioning, degradation, and transport behaviour demands sensitive and selective analytical methods for this complex mixture of up to 209 theoretically possible compounds. Congener-specific separation by high-resolution gas chromatography coupled with mass-selective detection would be a suitable approach to this multi-compound problem. In this paper, the separation of PCB congeners by capillary gas chromatography (HRGC) on a 50% n-octyl-methylpolysiloxane phase is presented.

  16. Lanthanide and actinide extractions with anionic ligands based on cobalt bis(dicarbollide) ions with covalently bonded CMPO functions

    Energy Technology Data Exchange (ETDEWEB)

    Selucky, P.; Rais, J.; Lucanikova, M. [Nuclear Research Inst. plc., Rez near Prague (Czech Republic); Gruener, B.; Kvicalova, M. [Inst. of Inorganic Chemistry, v.v.i., Academy of Sciences of the Czech Republic, Husinec-Rez near Prague (Czech Republic); Fejfarova, K. [Inst. of Physics, Academy of Sciences of the Czech Republic, Prague (Czech Republic); Cisarova, I. [Charles Univ., Prague (Czech Republic). Dept. of Chemistry

    2008-07-01

    Compounds were synthesized with the aim to develop efficient extraction agents for liquid-liquid extraction of polyvalent cations, i.e. lanthanides and actinides from high-level activity nuclear waste. Compounds of general formulation [(8-CMPO-(CH{sub 2}-CH{sub 2}O){sub 2}-1,2-C{sub 2}B{sub 9}H{sub 10})(1',2'-C{sub 2}B{sub 9}H{sub 11})-3.3'-Co(III)] with different phosphorus and nitrogen substitution (CMPO={sup 2}R,{sup 3}R P(O)-(CH{sub 2}){sub n}C(O)N{sup 1}R, {sup 1}R = t-octyl, H, Ph, {sup 2}R=Ph, n-octyl, {sup 3}R=Ph, n = 1,2)-(4a to 4e), were prepared and characterized by combination of {sup 11}B NMR, {sup 1}H high field NMR, ESI-M.S., HPLC and other techniques. Molecular structure of the sodium complex of ligand 4a ({sup 1}R = t-octyl, {sup 2}R = {sup 3}R = Ph, n = 1) was determined by single crystal X-ray diffraction analysis. Effect of several modifications in the structure of 4a-4e on the extraction properties was outlined. The study resulted in the definition of ionic ligand with enhanced extraction efficiency for 4a,b (t-octyl and H on the amidic nitrogen atom) and a better solubility of 4a and 4d ({sup 1}R = t-octyl, {sup 2}R = n-Oct, {sup 1}R=Ph, n = 1) in less polar solvents. Low polar mixtures of hydrogenated tetrapropylene (TPH) hexyl methyl ketone (HMK) can be applied as an auxiliary solvent for 4a, selected for detailed studies, replacing thus the polar and less environmentally friendly nitro-, fluoro- and chloro- solvents used in the current dicarbollide liquid-liquid extraction process. Results of the fission products separation from the simulated PUREX feed using 4a are presented inclusive procedures for Eu{sup 3+} stripping. (orig.)

  17. Proteomic changes in brain tissues of marine medaka (Oryzias melastigma) after chronic exposure to two antifouling compounds: Butenolide and 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT)

    KAUST Repository

    Chen, Lianguo

    2014-12-01

    SeaNine 211 with active ingredient of 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) has been used as a "green" antifouling agent worldwide but has raised serious biosafety concerns in coastal environments. DCOIT has the potential to disrupt the neurotransmission in nervous system, but the underlying mechanism has not been clarified. In the present study, we used TMT six-plex labeling coupled with two-dimensional LC-MS/MS analysis to investigate the protein expression profiles in brain tissues of the marine medaka (Oryzias melastigma) after a 28-day exposure to environmentally-realistic concentration of DCOIT at 2.55. μg/L (0.009. μM) or butenolide, one promising antifouling compound, at 2.31. μg/L (0.012. μM). DCOIT and butenolide induced differential expression of 26 and 18 proteins in male brains and of 27 and 23 proteins in female brains, respectively. Distinct mechanisms of toxicity were initiated by DCOIT and butenolide in males, whereas the protein expression profiles were largely similar in females treated by these two compounds. In males, DCOIT exposure mainly led to disruption of mitogen-activated protein kinase (MAPK) signaling pathway, while butenolide affected proteins related to the cytoskeletal disorganization that is considered as a general response to toxicant stress. Furthermore, a sex-dependent protein expression profile was also noted between male and female fish, as evident by the inverse changes in the expressions of common proteins (5 proteins for butenolide- and 2 proteins for DCOIT-exposed fish). Overall, this study provided insight into the molecular mechanisms underlying the toxicity of DCOIT and butenolide. The extremely low concentrations used in this study highlighted the ecological relevance, arguing for thorough assessments of their ecological risks before the commercialization of any new antifouling compound.

  18. Comparative safety of the antifouling compound butenolide and 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) to the marine medaka (Oryzias melastigma)

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lianguo [Division of Life Science, Hong Kong University of Science and Technology, Clear Water Bay, Hong Kong Special Administrative Region (Hong Kong); Ye, Rui [State Key Laboratory in Marine Pollution, Department of Biology and Chemistry, City University of Hong Kong, Kowloon, Hong Kong Special Administrative Region (Hong Kong); Xu, Ying; Gao, Zhaoming [Division of Life Science, Hong Kong University of Science and Technology, Clear Water Bay, Hong Kong Special Administrative Region (Hong Kong); Au, Doris W.T. [State Key Laboratory in Marine Pollution, Department of Biology and Chemistry, City University of Hong Kong, Kowloon, Hong Kong Special Administrative Region (Hong Kong); Qian, Pei-Yuan, E-mail: boqianpy@ust.hk [Division of Life Science, Hong Kong University of Science and Technology, Clear Water Bay, Hong Kong Special Administrative Region (Hong Kong)

    2014-04-01

    Highlights: • Adverse effects of antifouling compound butenolide were studied using marine medaka. • The active ingredient in SeaNine 211, DCOIT, was employed as positive control. • Butenolide induced transient, reversible biological effects on marine medaka. • Lower toxicity of butenolide on marine biota highlights its promising application. • The increased sensitivity of male medaka addresses the gender difference. - Abstract: This study evaluated the potential adverse effects of butenolide, a promising antifouling compound, using the marine medaka (Oryzias melastigma), a model fish for marine ecotoxicology. The active ingredient used in the commercial antifoulant SeaNine 211, 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) was employed as the positive control. Adult marine medaka (4-month-old) were exposed to various concentrations of butenolide or DCOIT for 28 days and then depurated in clean seawater for 14 days (recovery). A suite of sensitive biomarkers, including hepatic oxidative stress, neuronal signal transmission, endocrine disruption, and reproductive function, was used to measure significant biological effects induced by the chemicals. Compared to DCOIT, chronic exposure to butenolide induced a lower extent of oxidative stress in the liver of male and female medaka. Furthermore, butenolide-exposed fish could recover faster from oxidative stress than fish exposed to DCOIT. Regarding neurotransmission, DCOIT significantly inhibited acetylcholinesterase (AChE) activity in the brain of both male and female medaka, whereas this was not significant for butenolide. In addition, plasma estradiol (E{sub 2}) level was elevated and testosterone (T) level was decreased in male medaka exposed to DCOIT. This greatly imbalanced sex hormones ratio (E{sub 2}/T) in exposed males, indicating that DCOIT is a potent endocrine disruptive chemical. In contrast, butenolide induced only moderate effects on sex hormone levels in exposed males, which could be

  19. Comparative safety of the antifouling compound butenolide and 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) to the marine medaka (Oryzias melastigma)

    International Nuclear Information System (INIS)

    Chen, Lianguo; Ye, Rui; Xu, Ying; Gao, Zhaoming; Au, Doris W.T.; Qian, Pei-Yuan

    2014-01-01

    Highlights: • Adverse effects of antifouling compound butenolide were studied using marine medaka. • The active ingredient in SeaNine 211, DCOIT, was employed as positive control. • Butenolide induced transient, reversible biological effects on marine medaka. • Lower toxicity of butenolide on marine biota highlights its promising application. • The increased sensitivity of male medaka addresses the gender difference. - Abstract: This study evaluated the potential adverse effects of butenolide, a promising antifouling compound, using the marine medaka (Oryzias melastigma), a model fish for marine ecotoxicology. The active ingredient used in the commercial antifoulant SeaNine 211, 4,5-dichloro-2-n-octyl-4-isothiazolin-3-one (DCOIT) was employed as the positive control. Adult marine medaka (4-month-old) were exposed to various concentrations of butenolide or DCOIT for 28 days and then depurated in clean seawater for 14 days (recovery). A suite of sensitive biomarkers, including hepatic oxidative stress, neuronal signal transmission, endocrine disruption, and reproductive function, was used to measure significant biological effects induced by the chemicals. Compared to DCOIT, chronic exposure to butenolide induced a lower extent of oxidative stress in the liver of male and female medaka. Furthermore, butenolide-exposed fish could recover faster from oxidative stress than fish exposed to DCOIT. Regarding neurotransmission, DCOIT significantly inhibited acetylcholinesterase (AChE) activity in the brain of both male and female medaka, whereas this was not significant for butenolide. In addition, plasma estradiol (E 2 ) level was elevated and testosterone (T) level was decreased in male medaka exposed to DCOIT. This greatly imbalanced sex hormones ratio (E 2 /T) in exposed males, indicating that DCOIT is a potent endocrine disruptive chemical. In contrast, butenolide induced only moderate effects on sex hormone levels in exposed males, which could be gradually

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

    Directory of Open Access Journals (Sweden)

    Navabeh Nami

    2012-01-01

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

  1. Discovery of inhibitors of Leishmania β-1,2-mannosyltransferases using a click-chemistry-derived guanosine monophosphate library.

    Directory of Open Access Journals (Sweden)

    Phillip van der Peet

    Full Text Available Leishmania spp. are a medically important group of protozoan parasites that synthesize a novel intracellular carbohydrate reserve polymer termed mannogen. Mannogen is a soluble homopolymer of β-1,2-linked mannose residues that accumulates in the major pathogenic stages in the sandfly vector and mammalian host. While several steps in mannogen biosynthesis have been defined, none of the enzymes have been isolated or characterized. We report the development of a simple assay for the GDP-mannose-dependent β-1,2-mannosyltransferases involved in mannogen synthesis. This assay utilizes octyl α-D-mannopyranoside to prime the formation of short mannogen oligomers up to 5 mannose residues. This assay was used to screen a focussed library of 44 GMP-triazole adducts for inhibitors. Several compounds provided effective inhibition of mannogen β-1,2-mannosyltransferases in a cell-free membrane preparation. This assay and inhibitor compounds will be useful for dissecting the role of different mannosyltransferases in regulating de novo biosynthesis and elongation reactions in mannogen metabolism.

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

    Directory of Open Access Journals (Sweden)

    Hong-lin Zhu

    2011-07-01

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

  3. 2-[4-(2-Chloroacetylphenyl]-2-methyl-1-(pyrrolidin-1-ylpropan-1-one

    Directory of Open Access Journals (Sweden)

    Dong-mei Ren

    2013-08-01

    Full Text Available The asymmetric unit of the title compound, C16H20ClNO2, contains two molecules in which the dihedral angles between the benzene ring and the plane of the amide unit are 77.4 (1 and 81.1 (1°. In both molecules, the five-membered ring adopts an envelope conformation with one of the β-C atoms as the flap. In the crystal, molecules are connected via C—H...O hydrogen bonds, forming chains along the b-axis direction. These chains are further linked by C—H...π interactions, forming a three-dimensional network.

  4. Novel 1H-1,2,3-, 2H-1,2,3-, 1H-1,2,4- and 4H-1,2,4-triazole derivatives: a patent review (2008 - 2011).

    Science.gov (United States)

    Ferreira, Vitor F; da Rocha, David R; da Silva, Fernando C; Ferreira, Patrícia G; Boechat, Núbia A; Magalhães, Jorge L

    2013-03-01

    The triazoles represent a class of five-membered heterocyclic compounds of great importance for the preparation of new drugs with diverse biological activities because they may present several structural variations with the same numbers of carbon and nitrogen atoms. Due to the success of various triazoles that entered the pharmaceutical market and are still being used in medicines, many companies and research groups have shown interest in developing new methods of synthesis and biological evaluation of potential uses for these compounds. In this review, the authors explored aspects of patents for the 1H-1,2,3-, 2H-1,2,3-, 1H-1,2,4- and 4H-1,2,4-triazole families, including prototypes being considered in clinical studies between 2008 and 2011. The triazoles have been studied for over a century as an important class of heterocyclic compounds and still attract considerable attention due to their broad range of biological activities. More recently, there has been considerable interest in the development of novel triazoles with anti-inflammatory, antiplatelet, antimicrobial, antimycobacterial, antitumoral and antiviral properties and activity against several neglected diseases. This review emphasizes recent perspective and advances in the therapeutically active 1H-1,2,3-, 2H-1,2,3-, 1H-1,2,4- and 4H-1,2,4-triazole derivative patents between 2008 and 2011, covering the development of new chemical entities and new pharmaceuticals. Many studies have focused on these compounds as target structures and evaluated them in several biological targets. The preparation of 1H-1,2,3-, 2H-1,2,3-, 1H-1,2,4- and 4H-1,2,4-triazole derivatives brings to light several issues. There is a need to find new, more efficient preparations for these triazoles that take into consideration current issues in green chemistry, energy saving and sustainability. New diseases are discovered and new viruses and bacteria continue to challenge mankind, so it is imperative to find new prototypes for these

  5. Exploration of acetanilide derivatives of 1-(ω-phenoxyalkyl)uracils as novel inhibitors of Hepatitis C Virus replication.

    Science.gov (United States)

    Magri, Andrea; Ozerov, Alexander A; Tunitskaya, Vera L; Valuev-Elliston, Vladimir T; Wahid, Ahmed; Pirisi, Mario; Simmonds, Peter; Ivanov, Alexander V; Novikov, Mikhail S; Patel, Arvind H

    2016-07-12

    Hepatitis C Virus (HCV) is a major public health problem worldwide. While highly efficacious directly-acting antiviral agents have been developed in recent years, their high costs and relative inaccessibility make their use limited. Here, we describe new 1-(ω-phenoxyalkyl)uracils bearing acetanilide fragment in 3 position of pyrimidine ring as potential antiviral drugs against HCV. Using a combination of various biochemical assays and in vitro virus infection and replication models, we show that our compounds are able to significantly reduce viral genomic replication, independently of virus genotype, with their IC50 values in the nanomolar range. We also demonstrate that our compounds can block de novo RNA synthesis and that effect is dependent on a chemical structure of the compounds. A detailed structure-activity relationship revealed that the most active compounds were the N(3)-substituted uracil derivatives containing 6-(4-bromophenoxy)hexyl or 8-(4-bromophenoxy)octyl fragment at N(1) position.

  6. Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

    2016-10-01

    A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Hydrolyses of 2- and 4-fluoro N-heterocycles. 3. Nucleophilic catalysis by buffer bases in the general acid catalyzed hydrolysis of 4-fluoroquinaldine

    International Nuclear Information System (INIS)

    Muscio, O.J. Jr.; Theobald, P.G.; Rutherford, D.R.

    1989-01-01

    Pseudo-first-order rate constants and catalytic rate constants are reported for the buffer-catalyzed hydrolysis of 4-fluoroquinaldine (1) in carboxylic acid and phosphoric acid buffers. The buffer catalysis is consistent with specific acid, general base catalysis. Hydrolyses in 99% 18 O-labeled acetate, indicate that the predominant catalytic mode for the acetic acid/acetate buffer system is nucleophilic catalysis by the acetate anion coupled with specific acid catalysis. The other buffers presumably react in a similar manner. A Broensted-type plot of the catalytic rate constants for hydrolysis of protonated 1 has a slope of 0.57, with formate deviating positively from the line determined by acetate, chloroacetate, monohydrogen phosphate, and water. This Broensted slope is less than that found for hydrolysis of the 2-fluoro-1-methylpyridinium ion, 2, but is still within the range expected for aromatic nucleophilic substitution. Rate constants and 18 O-labeling results for hydrolysis in acetate buffer are also reported for 4-acetoxyquinaldine (3), the proposed intermediate in the acetate-catalyzed hydrolysis of 1. 15 references, 5 figures, 3 tables

  8. Spectral Analysis of 3-(Adamantan-1-yl)-4-Ethyl-1-[(4-Phenylpiperazin-1-yl) Methyl]-1 H-1,2,4-Triazole-5(4 H)-Thione

    Science.gov (United States)

    Mindarava, Y. L.; Shundalau, M. B.; Al-Wahaibi, L. H.; El-Emam, A. A.; Matsukovich, A. S.; Gaponenko, S. V.

    2018-05-01

    Vibrational IR (3200-650 cm-1) and Raman spectra (3200-150 cm-1) of adamantane-containing 3-(adamantan-1-yl)-4-ethyl-1-[(4-phenylpiperazin-1-yl)methyl]-1H-1,2,4-triazole-5(4H)-thione, which is promising for drug design, were examined. The UV/Vis spectrum (450-200 nm) of the compound in EtOH was measured. Full geometry optimization using density functional theory (DFT) in the B3LYP/cc-pVDZ approximation allowed the equilibrium configuration of the molecule to be determined and IR and Raman spectra to be calculated. Based on these, the experimental vibrational IR and Raman spectra were interpreted and the biological activity indices were predicted. The UV/Vis spectrum of the title compound was simulated at the time-dependent DFT/CAM-B3LYP/cc-pVDZ level with and without solvent effects and at the ab initio multi-reference perturbation theory XMCQDPT2 level. The UV/Vis spectrum that was simulated using the multi-reference XMCQDPT2 approximation agreed very successfully with the experimental data, in contrast to the single-reference DFT method. This was probably a consequence of intramolecular charge transfer.

  9. Spectral Analysis of 3-(Adamantan-1-yl)-4-Ethyl-1-[(4-Phenylpiperazin-1-yl) Methyl]-1H-1,2,4-Triazole-5(4H)-Thione

    Science.gov (United States)

    Mindarava, Y. L.; Shundalau, M. B.; Al-Wahaibi, L. H.; El-Emam, A. A.; Matsukovich, A. S.; Gaponenko, S. V.

    2018-05-01

    Vibrational IR (3200-650 cm-1) and Raman spectra (3200-150 cm-1) of adamantane-containing 3-(adamantan-1-yl)-4-ethyl-1-[(4-phenylpiperazin-1-yl)methyl]-1H-1,2,4-triazole-5(4H)-thione, which is promising for drug design, were examined. The UV/Vis spectrum (450-200 nm) of the compound in EtOH was measured. Full geometry optimization using density functional theory (DFT) in the B3LYP/cc-pVDZ approximation allowed the equilibrium configuration of the molecule to be determined and IR and Raman spectra to be calculated. Based on these, the experimental vibrational IR and Raman spectra were interpreted and the biological activity indices were predicted. The UV/Vis spectrum of the title compound was simulated at the time-dependent DFT/CAM-B3LYP/cc-pVDZ level with and without solvent effects and at the ab initio multi-reference perturbation theory XMCQDPT2 level. The UV/Vis spectrum that was simulated using the multi-reference XMCQDPT2 approximation agreed very successfully with the experimental data, in contrast to the single-reference DFT method. This was probably a consequence of intramolecular charge transfer.

  10. Pulsed laser thin film growth of di-octyl substituted polyfluorene and its co-polymers

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, R.K.; Ghosh, K.; Kahol, P.K. [Department of Physics, Astronomy and Materials Science, Missouri State University, Springfield, MO 65897 (United States); Yoon, J. [Department of Physics and Astronomy, University of Missouri, Columbia, MO 65211 (United States); Guha, S. [Department of Physics and Astronomy, University of Missouri, Columbia, MO 65211 (United States)], E-mail: guhas@missouri.edu

    2008-08-30

    Matrix-assisted pulsed laser deposition (PLD) allows a controlled layer-by-layer growth of polymer films. Di-octyl substituted polyfluorene (PF8) and its copolymers were deposited as thin films using matrix-assisted PLD by employing a KrF excimer laser with a fluence of 125 mJ/pulses. The optical and structural properties of these films are compared with spincoated films via Raman spectroscopy, absorption and photoluminescence. The Raman spectra of both PLD and spincoated films are similar indicating that the polymer films deposited via PLD maintain their molecular structure. Both the spincoated and the PLD grown PF8 films that were cast from toluene show the presence of the {beta} phase. Benzothiadiazole substituted PF8 (F8BT) and butyl phenyl-substituted PF8 (PFB) PLD grown films show a slightly broader emission compared to the spincoated films, which is attributed to an enhanced intermolecular interaction in the PLD grown thin films.

  11. Pulsed laser thin film growth of di-octyl substituted polyfluorene and its co-polymers

    International Nuclear Information System (INIS)

    Gupta, R.K.; Ghosh, K.; Kahol, P.K.; Yoon, J.; Guha, S.

    2008-01-01

    Matrix-assisted pulsed laser deposition (PLD) allows a controlled layer-by-layer growth of polymer films. Di-octyl substituted polyfluorene (PF8) and its copolymers were deposited as thin films using matrix-assisted PLD by employing a KrF excimer laser with a fluence of 125 mJ/pulses. The optical and structural properties of these films are compared with spincoated films via Raman spectroscopy, absorption and photoluminescence. The Raman spectra of both PLD and spincoated films are similar indicating that the polymer films deposited via PLD maintain their molecular structure. Both the spincoated and the PLD grown PF8 films that were cast from toluene show the presence of the β phase. Benzothiadiazole substituted PF8 (F8BT) and butyl phenyl-substituted PF8 (PFB) PLD grown films show a slightly broader emission compared to the spincoated films, which is attributed to an enhanced intermolecular interaction in the PLD grown thin films

  12. Pulsed laser thin film growth of di-octyl substituted polyfluorene and its co-polymers

    Science.gov (United States)

    Gupta, R. K.; Ghosh, K.; Kahol, P. K.; Yoon, J.; Guha, S.

    2008-08-01

    Matrix-assisted pulsed laser deposition (PLD) allows a controlled layer-by-layer growth of polymer films. Di-octyl substituted polyfluorene (PF8) and its copolymers were deposited as thin films using matrix-assisted PLD by employing a KrF excimer laser with a fluence of 125 mJ/pulses. The optical and structural properties of these films are compared with spincoated films via Raman spectroscopy, absorption and photoluminescence. The Raman spectra of both PLD and spincoated films are similar indicating that the polymer films deposited via PLD maintain their molecular structure. Both the spincoated and the PLD grown PF8 films that were cast from toluene show the presence of the β phase. Benzothiadiazole substituted PF8 (F8BT) and butyl phenyl-substituted PF8 (PFB) PLD grown films show a slightly broader emission compared to the spincoated films, which is attributed to an enhanced intermolecular interaction in the PLD grown thin films.

  13. Novel Pyridinium Surfactants with Unsaturated Alkyl Chains : Aggregation Behavior and Interactions with Methyl Orange in Aqueous Solution

    NARCIS (Netherlands)

    Kuiper, Johanna M.; Buwalda, Rixt T.; Hulst, Ron; Engberts, Jan B.F.N.

    2001-01-01

    This paper presents the synthesis and a study of the aggregation behavior of 4-undecyl-1-methyl- and 4-undecenyl-1-methylpyridinium iodide surfactants. The effect of the position of the double bond in the alkyl chain of the surfactant on the critical micelle concentration (cmc), degree of counterion

  14. Synthesis and fungicidal activity of pyrazole derivatives containing 1,2,3,4-tetrahydroquinoline.

    Science.gov (United States)

    Lei, Peng; Zhang, Xuebo; Xu, Yan; Xu, Gaofei; Liu, Xili; Yang, Xinling; Zhang, Xiaohe; Ling, Yun

    2016-01-01

    Take-all of wheat, caused by the soil-borne fungus Gaeumannomyces graminis var. tritici, is one of the most important and widespread root diseases. Given that take-all is still hard to control, it is necessary to develop new effective agrochemicals. Pyrazole derivatives have been often reported for their favorable bioactivities. In order to discover compounds with high fungicidal activity and simple structures, 1,2,3,4-tetrahydroquinoline, a biologically active group of natural products, was introduced to pyrazole structure. A series of pyrazole derivatives containing 1,2,3,4-tetrahydroquinoline were synthesized, and their fungicidal activities were evaluated. The bioassay results demonstrated that the title compounds displayed obvious fungicidal activities at a concentration of 50 μg/mL, especially against V. mali, S. sclerotiorum and G. graminis var. tritici. The inhibition rates of compounds 10d, 10e, 10h, 10i and 10j against G. graminis var. tritici were all above 90 %. Even at a lower concentration of 16.7 μg/mL, compounds 10d and 10e exhibited satisfied activities of 100 % and 94.0 %, respectively. It is comparable to that of the positive control pyraclostrobin with 100 % inhibition rate. A series of pyrazole derivatives containing 1,2,3,4-tetrahydroquinoline were synthesized and their structures were confirmed by (1)H NMR, (13)C NMR, IR spectrum and HRMS or elemental analysis. The crystal structure of compound 10g was confirmed by X-ray diffraction. Bioassay results indicated that all title compounds exhibited obvious fungicidal activities. In particular, compounds 10d and 10e showed comparable activities against G. graminis var. tritici with the commercial fungicide pyraclostrobin at the concentration of 16.7 μg/mL.Graphical abstractA series of pyrazole derivatives containing 1,2,3,4-tetrahydroquinoline were designed and synthesized. Bioassay results indicated that all these compounds exhibited obvious fungicidal activities.

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

    Directory of Open Access Journals (Sweden)

    Yu. S. Hulina

    2017-02-01

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

  16. Self-Assembly, Surface Activity and Structure of n-Octyl-β-D-thioglucopyranoside in Ethylene Glycol-Water Mixtures

    Directory of Open Access Journals (Sweden)

    Cristóbal Carnero Ruiz

    2013-02-01

    Full Text Available The effect of the addition of ethylene glycol (EG on the interfacial adsorption and micellar properties of the alkylglucoside surfactant n-octyl-β-D-thioglucopyranoside (OTG has been investigated. Critical micelle concentrations (cmc upon EG addition were obtained by both surface tension measurements and the pyrene 1:3 ratio method. A systematic increase in the cmc induced by the presence of the co-solvent was observed. This behavior was attributed to a reduction in the cohesive energy of the mixed solvent with respect to pure water, which favors an increase in the solubility of the surfactant with EG content. Static light scattering measurements revealed a decrease in the mean aggregation number of the OTG micelles with EG addition. Moreover, dynamic light scattering data showed that the effect of the surfactant concentration on micellar size is also controlled by the content of the co-solvent in the system. Finally, the effect of EG addition on the microstructure of OTG micelles was investigated using the hydrophobic probe Coumarin 153 (C153. Time-resolved fluorescence anisotropy decay curves of the probe solubilized in micelles were analyzed using the two-step model. The results indicate a slight reduction of the average reorientation time of the probe molecule with increasing EG in the mixed solvent system, thereby suggesting a lesser compactness induced by the presence of the co-solvent.

  17. Flotation Behaviors of Perovskite, Titanaugite, and Magnesium Aluminate Spinel Using Octyl Hydroxamic Acid as the Collector

    Directory of Open Access Journals (Sweden)

    Weiqing Wang

    2017-08-01

    Full Text Available The flotation behaviors of perovskite, titanaugite, and magnesium aluminate spinel (MA-spinel, using octyl hydroxamic acid (OHA as the collector, were investigated using microflotation experiments, zeta-potential measurements, Fourier transform infrared (FT-IR analyses, X-ray photoelectron spectroscopy (XPS analyses, and flotation experiments on artificially mixed minerals. The microflotation experiments show that the floatability of perovskite is clearly better than titanaugite and MA-spinel at around pH 5.5, while titanaugite possesses certain floatability at pH 6.0–6.5, and MA-spinel displays good floatability at pH > 8.0. The results of the FT-IR and XPS analyses show that OHA mainly interacts with Ti, resulting in perovskite flotation, and that the Al on titanaugite, as well as the Mg and Al on the MA-spinel surface, chemically react with OHA under acidic conditions. However, OHA mainly reacts with the Ti and Ca on the perovskite surface, Ca and Mg on the titanaugite surface, and Mg and Al on the MA-spinel surface under alkaline conditions. The results of the artificially mixed mineral flotation experiment show that the concentrate of TiO2 grade increased from 19.73% to 30.18% at pH 5.4, which indicates that a weakly acidic solution is the appropriate condition for the flotation separation of perovskite from titanaugite and MA-spinel. The results of the modified slag flotation experiments show that the TiO2 grade of concentrate increased from 18.13% to 23.88% at pH 5.4, through the open circuit test of “one roughing and one cleaning”. OHA displays selectivity toward perovskite in the modified slag flotation, but the consumption of H2SO4 is very high. The CaSO4 precipitate covered on the mineral surfaces results in poor TiO2 grade and recovery.

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

    Science.gov (United States)

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

    2001-09-01

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

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

    Directory of Open Access Journals (Sweden)

    G. B. Venkatesh

    2014-12-01

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

  20. Laboratory scale investigations for testing the uptake potential of 1, 3 di octyloxy Calix(4)arene Crown 6 for separation of Cs from high level radioactive waste

    International Nuclear Information System (INIS)

    Thorat, Vidya; Soudamini, N.; Achare, Sanjay; Girisan, Prema; Mishra, R.K.; Kumar, Amar; Kaushik, C.P.; Banerjee, K.

    2016-01-01

    137 Cs one of the major beta gamma emitting fission products present in high level liquid waste (HLLW), which is generated during the reprocessing of spent nuclear fuel. Its separation will restrict the personal radiation exposure during the vitrification and prevents thermal deformation of conditioned waste matrix during storage. Separation will also reduce the volume of vitrified mass to be stored in repository. In addition 137 Cs has enormous applications as radiation sources in food preservation, sterilization of medical products, brachytherapy, blood irradiation, hygienization of sewage sludge etc. The use of 137 Cs (T 1/2 = 30 years) in place of 60 Co (T 1/2 = 5.2 years) will also reduce the shielding requirement, frequency of source replenishment and ease the handling/transportation of radioactive source. Present paper summarises experimental results pertaining to performance evaluation of indigenously synthesised 1, 3 di octyl oxy Calix(4) arene crown 6 (CC6) as extractant for recovery of caesium from HLLW

  1. Synthesis and Cytotoxic Evaluation of 1H-1,2,3-Triazol-1-ylmethyl-2,3-dihydronaphtho[1,2-b]furan-4,5-diones

    Directory of Open Access Journals (Sweden)

    INGRID C. CHIPOLINE

    2018-02-01

    Full Text Available ABSTRACT The 1,2-naphthoquinone compound was previously considered active against solid tumors. Moreover, glycosidase inhibitors such as 1,2,3-1H triazoles has been pointed out as efficient compounds in anticancer activity studies. Thus, a series of eleven 1,2-naphthoquinones tethered in C2 to 1,2,3-1H-triazoles 9a-k were designed, synthesized and their cytotoxic activity evaluated using HCT-116 (colon adenocarcinoma, MCF-7 (breast adenocarcinoma and RPE (human nontumor cell line from retinal epithelium. The chemical synthesis was performed from C-3 allylation of lawsone followed by iodocyclization with subsequent nucleophilic displacement with sodium azide and, finally, the 1,3-dipolar cycloaddition catalyzed by Cu(I with terminal alkynes led to the formation of 1H-1,2,3-Triazol-1-ylmethyl-2,3-dihydronaphtho[1,2-b]furan-4,5-diones in good yields. Compounds containing aromatic group linked to 1,2,3-triazole ring (9c, 9d, 9e, 9i presented superior cytotoxic activity against cancer cell lines with IC50 in the range of 0.74 to 4.4 µM indicating that the presence of aromatic rings substituents in the 1,2,3-1H-triazole moiety is probably responsible for the improved cytotoxic activity.

  2. Regioselectivity in the Thermal Rearrangement of Unsymmetrical 4-Methyl-4H-1,2,4-triazoles to 1-Methyl-1H-1,2,4-triazoles

    Directory of Open Access Journals (Sweden)

    Per H.J. Carlsen

    2001-11-01

    Full Text Available The rearrangement of 4-methyl-3,5-diaryl-4H-1,2,4-triazoles to the corresponding 1-methyl-3,5-diaryl-1H-1,2,4-triazoles showed regioselectivity comparable to that observed for the alkylation of 3,5-diaryl-1H-1,2,4-triazoles. This lends support to a proposed mechanism for the rearrangement that involves consecutive nucleophilic displacements steps.

  3. Synthesis and reactions of diazocarbonyl compounds. I. Reaction of 1-diazo-3-, 1-diazo-4-, and 1-diazo-5-phthalimidoalkan-2-ones with hydrazine hydrate. Synthesis of 1-diazo-3-, 1-diazo-4, and 1-diazo-5-arenesulfamoyl-alkan-2-ones

    International Nuclear Information System (INIS)

    Sipyagin, A.M.; Kartsev, V.G.

    1986-01-01

    The reaction of hydrazine hydrate with 1-diazo-3-, 1-diazo-4-, and 1-diazo-5-phthalimidoalkan-2-ones containing a substituent at the α position to the phthalimide group in the hydrocarbon chain leads to the formation of 1-diazo-3- and 1-diazo-4-(2-hydrazidophenylcarbamoyl)alkan-2-ones. On heating in the presence of an excess of hydrazine hydrate the reaction products are 1-diazo-3-, 1-diazo-4-, and 1-diazo-5-aminoalkan-2-ones. Various 1-diazo-3-, 1-diazo-4-, and 1-diazo-5-arenesulfamoyl-alkan-2-ones were synthesized in the reaction of arenesulfonyl chlorides with 1-diazo-3-, 1-diazo-4-, and 1-diazo-5-aminoalkan-2-ones in the presence of triethylamine

  4. Thermochemistry of organic azides revisited

    International Nuclear Information System (INIS)

    Emel'yanenko, Vladimir N.; Algarra, Manuel; Esteves da Silva, Joaquim C.G.; Hierrezuelo, Jesús; López-Romero, Juan M.; Verevkin, Sergey P.

    2014-01-01

    Highlights: • Pure samples of 4-nitro-phenyl azide, 1-octyl- and 1-decyl-azides were prepared. • Vapour pressures, sublimation and vaporization enthalpies measured by transpiration. • Enthalpy of formation of 1-alkyl azides measured by combustion calorimetry. • Enthalpy of fusion of 4-nitro-phenyl azide measured by DSC. • Experimental gas enthalpies of formation were in agreement with calculated by G4. - Abstract: Highly pure samples of 4-nitro-phenyl azide, 1-octyl azide and 1 decyl-azide were prepared for thermochemical studies. Vapour pressures over the solid and the liquid sample of 4-nitro-phenyl azide have been determined by the transpiration method. The molar enthalpies of vaporization/sublimation for this compound were derived from the temperature dependencies of vapour pressures. The molar enthalpy of fusion of 4-nitro-phenyl azide was measured by DSC. The measured data set for 4-nitro-phenyl azide was successfully checked for internal consistency. Molar enthalpies of vaporization of 1-octyl azide and 1 decyl-azide were measured by transpiration. The molar enthalpies of formation of the liquid 1-octyl azide and 1 decyl-azides were derived from the combustion calorimetry. New experimental results for these organic azides have been used to derive their molar enthalpies of formation in the gas state and for comparison with results from quantum-chemical method G4

  5. Metabolism of 1,2,3,4-, 1,2,3,5-, and 1,2,4,5-tetrachlorobenzene in the squirrel monkey

    International Nuclear Information System (INIS)

    Schwartz, H.; Chu, I.; Villeneuve, D.C.; Benoit, F.M.

    1987-01-01

    The metabolism of three tetrachlorobenzene isomers (TeCB) was investigated in the squirrel monkey. The animals were administered orally 6 single doses of 14 C-labeled 1,2,3,4-, 1,2,4,5-, or 1,2,3,5-tetrachlorobenzene over a 3-wk period at levels ranging from 50 to 100 mg/kg body weight (b.w) and kept in individual metabolism cages to collect urine and feces for radioassay. Approximately 38% (1,2,3,4-TeCB), 36% (1,2,3,5-TeCB), and 18% (1,2,4,5-TeCB) of the doses were excreted respectively in the feces 48 h post administration. In monkeys dosed with 1,2,3,4-TeCB, unchanged compound accounted for 50% of the fecal radioactivity. Unchanged compound accounted for more than 50% of the fecal radioactivity found in the monkeys dosed with 1,2,3,5-TeCB. The fecal metabolites were identified in both groups. No metabolites were detected in the feces of monkeys dosed with 1,2,4,5-TeCB. While the fecal route represented the major route of excretion for 1,2,3,4-TeCB, the other two isomers were eliminated exclusively in the feces. The above data in the squirrel monkey are different from those obtained with the rat and the rabbit, and demonstrate the different metabolic pathways for the isomers

  6. Environmentally benign synthesis of sydnone containing 1,3,4 ...

    Indian Academy of Sciences (India)

    TECS

    lop benign synthetic methods for sydnone deriva- tives,. 9 we report here a new series of sydnone containing 1,3,4-thiadiazines by microwave irradia- tion under solvent-free conditions. 2. Experimental. 2.1 General remarks. Melting points were determined by open capillary method and are uncorrected. All compounds were.

  7. Vicarious nucleophilic substitution to prepare 1,3-diamino-2,4,6-trinitrobenzene or 1,3,5-triamino-2,4,6-trinitrobenzene

    Science.gov (United States)

    Mitchell, Alexander R.; Pagoria, Philip F.; Schmidt, Robert D.

    1996-01-01

    The present invention relates to a process to produce 1,3-diamino-2,4,6-trinitrobenzene (DATB) or 1,3,5-triamino-2,4,6,-trinitrobenzene (TATB) by: (a) reacting at ambient pressure and a temperature of between about 0.degree. and 50.degree. C. for between about 0.1 and 24 hr, a trinitroaromatic compound of structure V: ##STR1## wherein X, Y, and Z are each independently selected from --H, or --NH.sub.2, with the proviso that at least 1 or 2 of X, Y, and Z are hydrogen, with an amount effective to produce DATB or TATB of 1,1,1-trialkylhydrazinium halide wherein alkyl is selected from methyl, ethyl, propyl or butyl and halide is selected from chloride, bromide or iodide. in the presence of a strong base selected from sodium butoxide, potassium butoxide, potassium propoxide, sodium propoxide, sodium ethoxide, potassium ethoxide, sodium methoxide, potassium methoxide, and combinations thereof; in a solvent selected from the group consisting of methanol, ethanol, propanol, butanol, dimethylsulphoxide, N-methylpyrrolidone, hexamethylphosphoramide, dimethylformide, dimethylacetamide and mixtures thereof, provided that when alcohols are present primarily DATB and picramide is formed; and (b) isolating the DATB or TATB produced. DATB and TATB are useful specialty explosives. TATB is also used for the preparation of benzenehexamine, a starting material for the synthesis of novel materials (optical imaging devices, liquid crystals, ferromagnetic compounds).

  8. Liquid scintillation solution

    International Nuclear Information System (INIS)

    Long, E.C.

    1976-01-01

    The invention deals with a liquid scintillation solution which contains 1) a scintillation solvent (toluol), 2) a primary scintillation solute (PPO), 3) a secondary scintillation solute (dimethyl POPOP), 4) several surfactants (iso-octyl-phenol polyethoxy-ethanol and sodium di-hexyl sulfosuccinate) essentially different from one another and 5) a filter resolution and/or transparent-making agent (cyclic ether, especially tetrahydrofuran). (HP) [de

  9. Fragrance material review on 1-[5(or 6)-methyl-7(or 8)-1-(methylethyl)bicyclo[2.2.2]oct-5-en-2-yl]ethan-1-one.

    Science.gov (United States)

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

    2013-12-01

    A toxicologic and dermatologic review of 1-[5(Or 6)-Methyl-7(or 8)-1-(methylethyl)bicyclo[2.2.2]oct-5-en-2-yl]ethan-1-one when used as a fragrance ingredient is presented. 1-[5(Or 6)-Methyl-7(or 8)-1-(methylethyl)bicyclo[2.2.2]oct-5-en-2-yl]ethan-1-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 1-[5(Or 6)-Methyl-7(or 8)-1-(methylethyl)bicyclo[2.2.2]oct-5-en-2-yl]ethan-1-one were evaluated then summarized and includes physical properties, acute toxicity, skin irritation, mucous membrane (eye) irritation, skin sensitization, phototoxicity, photoallergy, and genotoxicity, data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al., Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones When Used as Fragrance Ingredients. (submitted for publication)). for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

  10. The Effect of Quartz on the Flotation of Fine Wolframite with Octyl Hydroxamic Acid

    Directory of Open Access Journals (Sweden)

    Qingyou Meng

    2017-09-01

    Full Text Available The influence of quartz on the flotation of fine wolframite using octyl hydroxamic acid (OHA as the collector was investigated by micro-flotation tests, inductively coupled plasma (ICP measurements, adsorption experiments, zeta potential, and Fourier transform infrared spectroscopy (FT-IR analysis. Micro-flotation tests showed that a large difference in floatability existed between fine wolframite and quartz in the pH range of 7.0 to 10.0. However, in a synthetic mixture, the flotation separation of fine wolframite from quartz became more difficult as the particle size of the latter decreased. When a dissolved solution of wolframite was used as the flotation medium, quartz floatability improved significantly. Zeta potentials of quartz particles shifted positively in the dissolved solution of wolframite compared to distilled water, especially at a pH level of 7.0–10.0, which was attributed to the metal ions dissolved from the wolframite being adsorbed onto the quartz surface. The surface activation of quartz led to an increase in the OHA adsorption and made the surface hydrophobic. FT-IR analysis further demonstrated that OHA could adsorb onto the activated quartz surface through a dominantly chemical process.

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

    Science.gov (United States)

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

    2013-12-01

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

  12. 40 CFR 721.7160 - 2-Oxepanone, polymer with 4,4′-(1-methylethylidene)bisphenol and 2,2-[(1-methylethylidene)bis(4,1...

    Science.gov (United States)

    2010-07-01

    ...-methylethylidene)bisphenol and 2,2-[(1-methylethylidene)bis(4,1-phe-ny-lene-oxy-methyl-ene)]-bi-sox-i- rane, graft... Substances § 721.7160 2-Oxepanone, polymer with 4,4′-(1-methylethylidene)bisphenol and 2,2-[(1... new uses subject to reporting. (1) The chemical substance 2-oxepanone, polymer with 4,4′(1-meth-yl-eth...

  13. 4-Aminobenzoic acid–1,2-bis(4-pyridylethane (2/1

    Directory of Open Access Journals (Sweden)

    Fwu Ming Shen

    2010-07-01

    Full Text Available In the title compound, C12H12N2·2C7H7NO2, the 4-aminobenzoic acid molecules are linked by O—H...N hydrogen bonds to 1,2-bis(4-pyridylethane, forming linear hydrogen bonded chains parallel to [2overline{1}1]. The structure exhibits a hydrogen-bonding network involving COOH...N(pyridyl and amine and carboxylic N—H... O interactions. In addition, π–π stacking interactions [centroid–centroid distance = 3.8622 (14 Å] are also present.

  14. In situ electrochemical SFG/DFG study of CN- and nitrile adsorption at Au from 1-butyl-1-methyl-pyrrolidinium bis(trifluoromethylsulfonyl) amide ionic liquid([BMP][TFSA]) containing 4-{2-[1-(2-cyanoethyl)-1,2,3,4-tetrahydroquinolin-6-yl]diazenyl} benzonitrile (CTDB) and K[Au(CN)₂].

    Science.gov (United States)

    Bozzini, Benedetto; Busson, Bertrand; Gayral, Audrey; Humbert, Christophe; Mele, Claudio; Six, Catherine; Tadjeddine, Abderrahmane

    2012-06-25

    In this paper we report an in situ electrochemical Sum-/Difference Frequency Generation (SFG/DFG) spectroscopy investigation of the adsorption of nitrile and CN⁻ from the ionic liquid 1-butyl-1-methyl-pyrrolidinium bis(trifluoromethylsulfonyl) amide ([BMP][TFSA]) containing 4-{2-[1-(2-cyanoethyl)-1,2,3,4-tetrahydroquinolin-6-yl]-diazenyl}benzonitrile (CTDB) at Au electrodes in the absence and in the presence of the Au-electrodeposition process from K[Au(CN)₂]. The adsorption of nitrile and its coadsorption with CN⁻ resulting either from the cathodic decomposition of the dye or from ligand release from the Au(I) cyanocomplex yield potential-dependent single or double SFG bands in the range 2,125-2,140 cm⁻¹, exhibiting Stark tuning values of ca. 3 and 1 cm⁻¹ V⁻¹ in the absence and presence of electrodeposition, respectively. The low Stark tuning found during electrodeposition correlates with the cathodic inhibiting effect of CTDB, giving rise to its levelling properties. The essential insensitivity of the other DFG parameters to the electrodeposition process is due to the growth of smooth Au.

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

    Directory of Open Access Journals (Sweden)

    Baskar Nammalwar

    2013-12-01

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

  16. Studies in the stereoselective synthesis of 1,1-disubstituted 1,2,3,4-tetrahydroisoquinolines

    OpenAIRE

    Berg, Michael Arthur George

    1992-01-01

    Isoquinoline alkaloids and analogs play an important role in today's pharmaceutical industry. The need to synthesize single stereoisomers of these alkaloids is important. Many times only a single stereoisomer exhibits the desired activity, while other stereoisomers of the alkaloid exhibit undesired side effects. The stereoselective synthesis of 1, 1-disubstituted 1,2,3,4- tetrahydroisoquinolines using Reissert compound chemistry containing chiral acyl auxiliaries was studied with the ultimate...

  17. Crystal structures of bis[2-(pyridin-2-ylphenyl-κ2N,C1]rhodium(III complexes containing an acetonitrile or monodentate thyminate(1− ligand

    Directory of Open Access Journals (Sweden)

    Mika Sakate

    2016-04-01

    Full Text Available The crystal structures of bis[2-(pyridin-2-ylphenyl]rhodium(III complexes with the metal in an octahedral coordination containing chloride and acetonitrile ligands, namely (OC-6-42-acetonitrilechloridobis[2-(pyridin-2-ylphenyl-κ2N,C1]rhodium(III, [RhCl(C11H8N2(CH3CN] (1, thyminate(1− and methanol, namely (OC-6-42-methanol(5-methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-ido-κN1bis[2-(pyridin-2-ylphenyl-κ2N,C1]rhodium(III, [Rh(C11H8N2(C5H5N2O2(CH3OH]·CH3OH·0.5H2O (2, and thyminate(1− and ethanol, namely (OC-6-42-ethanol(5-methyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-1-ido-κN1bis[2-(pyridin-2-ylphenyl-κ2N,C1]rhodium(III, [Rh(C11H8N2(C5H5N2O2(C2H5OH]·C2H5OH (3, are reported. The acetonitrile complex, 1, is isostructural with the IrIII analog. In complexes 2 and 3, the monodeprotonated thyminate (Hthym− ligand coordinates to the RhIII atom through the N atom, and the resulting Rh—N(Hthym bond lengths are relatively long [2.261 (2 and 2.252 (2 Å for 2 and 3, respectively] as compared to the Rh—N bonds in the related thyminate complexes. In each of the crystals of 2 and 3, the complexes are linked via a pair of intermolecular N—H...O hydrogen bonds between neighbouring Hthym− ligands, forming an inversion dimer. A strong intramolecular O—H...O hydrogen bond between the thyminate(1− and alcohol ligands in mutually cis positions to each other is also observed.

  18. Development of a Novel Synthetic Drug for Osteoporosis and Fracture Healing

    Science.gov (United States)

    2014-09-01

    in situ curing at the fracture site. We are examining injectable hydrogel that is formed by reacting eight-arm poly(ethylene glycol ) thiol (PEG8SH...sec-butyl, 15 tert--butyl, pentyl, 2--pentyl, 3--penty1, neopentyl , hexy1, heptyl, octyl, and the Eke, and the corresponding groups containing one or

  19. Synthesis, physical and chemical properties, antihypoxic activity of some 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-N-R1-1,3,4-thiadiazole-2-amines and 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-4-R1-4H-1,2,4-t

    Directory of Open Access Journals (Sweden)

    V. M. Odyntsova

    2018-03-01

    Full Text Available Today, an increase of natural and technogenic situations leads to the disorders of the central nervous system, functional-metabolic processes, vascular diseases, in particular, acute cerebral blood flow disorders. In addition, the changes occurring on the molecular and cellular levels are in the basis of the functional violations of individual systems and the organism as a whole. Hypoxia not only complicates the disease course, but in most cases, determines its outcome. The important role in the fight against hypoxia belongs to antioxidants, which improve the circulating oxygen utilization by the body, reduce its need for the organs and tissues, which is not only expedient but necessary for the treatment of many acute and chronic pathological processes. So, the frequency of the hypoxic states and a wide range of factors causing them determine the relevance of new ways and methods finding to overcome the oxygen deficiency. The aim of this work is the purposeful search of some 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-N-R1-1,3,4-thiadiazole-2-amines and 5-[((5-(adamantane-1-yl-4-R-4H-1,2,4-triazole-3-ylthiomethyl]-4-R1-4H-1,2,4-triazole-3-thiols, the study of their physical and chemical properties and pharmacological screening of the antihypoxic activity of the obtained compounds. Materials and methods. The study of physical and chemical properties was conducted on certified and licensed modern equipment. Antihypoxic activity was studied during the modeling process of hypoxia with hypercapnia. Mexidol was used as a comparison drug in studies at a dose of 100 mg/kg. Results. As the result of the study, it was found that the synthesized compounds and the comparison drug influenced on rats’ life span differently. Compounds, the antihypoxic activity of which exceeded control have been discovered, and others’ were at the level of Mexidol. A number of compounds showed a somewhat less activity in comparison with control, and two

  20. Ionothermal synthesis, crystal structure, and magnetic study of Co2PO4OH isostructural with caminite.

    Science.gov (United States)

    Wang, Guangmei; Valldor, Martin; Spielberg, Eike T; Mudring, Anja-Verena

    2014-03-17

    A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

  1. Catalytic Upgrading of bio-oil using 1-octene and 1-butanol over sulfonic acid resin catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Zhijun; Wang, Qingwen; Tripathi, Prabhat; Pittman, Charles U.

    2011-02-04

    Raw bio-oil from fast pyrolysis of biomass must be refined before it can be used as a transporation fuel, a petroleum refinery feed or for many other fuel uses. Raw bio-oil was upgraded with the neat model olefin, 1-octene, and with 1-octene/1-butanol mixtures over sulfonic acid resin catalysts frin 80 to 150 degrees celisus in order to simultaneously lower water content and acidity and to increase hydrophobicity and heating value. Phase separation and coke formation were key factors limiting the reaction rate during upgrading with neat 1-octene although octanols were formed by 1-octene hydration along with small amounts of octyl acetates and ethers. GC-MS analysis confirmed that olefin hydration, carboxylic acid esterification, acetal formation from aldehydes and ketones and O- and C-alkylations of phenolic compounds occurred simultaneously during upgrading with 1-octene/1-butanol mixtures. Addition of 1-butanol increased olefin conversion dramatically be reducing mass transfer restraints and serving as a cosolvent or emulsifying agent. It also reacted with carboxylic acids and aldehydes/ketones to form esters, and acetals, respectively, while also serving to stabilize bio-oil during heating. 1-Butanol addition also protected the catalysts, increasing catalyst lifetime and reducing or eliminationg coking. Upgrading sharply increased ester content and decreased the amounts of levoglucosan, polyhydric alcohols and organic acids. Upgrading lowered acidity (pH value rise from 2.5 to >3.0), removed the uppleasant ordor and increased hydrocarbon solubility. Water content decreased from 37.2% to < 7.5% dramatically and calorific value increased from 12.6 MJ kg to about 30.0 MJ kg.

  2. Synthesis, antimicrobial, and anti-inflammatory activities of novel 2-[3-(1-adamantyl)-4-substituted-5-thioxo-1,2,4-triazolin-1-yl] acetic acids, 2-[3-(1-adamantyl)-4-substituted-5-thioxo-1,2,4-triazolin-1-yl]propionic acids and related derivatives.

    Science.gov (United States)

    Al-Deeb, Omar A; Al-Omar, Mohamed A; El-Brollosy, Nasser R; Habib, Elsayed E; Ibrahim, Tarek M; El-Emam, Ali A

    2006-01-01

    The reaction of 3-(1-adamantyl)-4-substituted-1,2,4-triazoline-5-thiones 3a-g with sodium chloroacetate, in ethanolic sodium hydroxide yielded the corresponding N1-acetic acid derivatives 4a-g. The interaction of 3a-g with ethyl 2-bromopropionate in acetone, in the presence of potassium carbonate, yielded the corresponding N1-ethyl propionate derivatives 5a-g, which upon hydrolysis with aqueous sodium hydroxide afforded the corresponding propionic acid derivatives 6a-g. Similarly, the reaction of 3-(1-adamantyl)-4-amino-1,2,4-triazoline-5-thione 7 with sodium chloroacetate in ethanolic sodium hydroxide yielded the corresponding N1-acetic acid derivative 8. On the other hand, the reaction of 2-(1-adamantyl)-1,3,4-oxadiazoline-5-thione 9 with sodium chloroacetate yielded the corresponding S-acetic acid derivative 10. Compounds 4a-g, 5b, 5c, 5g, 6a-g, 8 and 10 were tested for in vitro activities against a panel of Gram-positive and Gram-negative bacteria and the yeast-like pathogenic fungus Candida albicans. Several derivatives produced good or moderate activities particularly against Bacillus subtilis. In addition, the in vivo anti-inflammatory activities of these compounds were determined using the carrageenin-induced paw oedema method in rats. Compounds 4a, 4b, 4e, 4f, 6f, 6g and 10 produced good dose-dependent anti-inflammatory activities.

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

    Directory of Open Access Journals (Sweden)

    Allaoua Kedjadja

    2015-10-01

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

  4. Residual stresses in 2 1/4Cr1Mo welds

    International Nuclear Information System (INIS)

    Fidler, R.; Jerram, K.

    1978-01-01

    Two separate investigations, initiated in an attempt to explain the large amount of residual stress scatter previously observed in the weld metal of eighteen nominally identical thick-section 2 1/4Cr1Mo butt welds, are described in this paper. The first examined the detailed surface residual stress distributions in 2 1/4Cr1Mo manual arc circumferential butt welds in 80mm and 100mm thick 1/2Cr1/2Mo1/4V steam pipe. High residual stresses were found in the regions of overlap between adjacent weld beads, with low values in virgin weld metal. The second utilised single pass manual metal arc bead-in-groove welds to investigate the effects of preheat and weld metal composition on weld metal residual stresses. In four weld metals, mild steel, 1/2Cr1/2Mo1/4V, 1Cr1/2Mo, and 2 1/4Cr1Mo, the residual stresses were very similar, becoming less tensile (or more compressive) with increase of preheat, while the residual stresses in the fifth weld metal (12Cr) were significantly different, being compressive and less affected by preheat. In both investigations the effects have been described in terms of the basic metallurgical phenomena occurring in the weld metal. (author)

  5. 6,6'-(1E,1'E-((1R,2R-1,2-Diphenylethane-1,2-diylbis(azan-1-yl-1-ylidenebis(methan-1-yl-1-ylidenebis(2-tert-butyl-4-((trimethylsilylethynylphenol

    Directory of Open Access Journals (Sweden)

    David Díaz Díaz

    2013-03-01

    Full Text Available Functionalizable salen derivative, 6,6'-(1E,1'E-((1R,2R-1,2-diphenylethane-1,2-diylbis(azan-1-yl-1-ylidenebis(methan-1-yl-1-ylidenebis(2-tert-butyl-4-((trimethylsilyl ethyn-ylphenol (3, was synthesized by condensation between (1R,2R-1,2-diphenylethane-1,2-diamine (2 and 3-tert-butyl-2-hydroxy-5-((trimethylsilylethynyl benzaldehyde (1 under refluxing conditions. The title compound was characterized by 1H-NMR, 13C-NMR, FT-IR, high-resolution mass spectrometry, optical rotation and melting point determination.

  6. Inhibition of Procarcinogen Activating Enzyme CYP1A2 Activity and Free Radical Formation by Caffeic Acid and its Amide Analogues.

    Science.gov (United States)

    Narongchai, Paitoon; Niwatananun, Kanokporn; Narongchai, Siripun; Kusirisin, Winthana; Jaikang, Churdsak

    2016-01-01

    Caffeic acid (CAF) and its amide analogues, ethyl 1-(3',4'-dihydroxyphenyl) propen amide (EDPA), phenethyl 1-(3',4'-dihydroxyphenyl) propen amide (PEDPA), phenmethyl 1- (3',4'-dihydroxyphenyl) propen amide (PMDPA) and octyl 1-(3',4'-dihydroxyphenyl) propen amide (ODPA) were investigated for the inhibition of procarcinogen activating enzyme. CYP1A2 and scavenging activity on formation of nitric oxide, superoxide anion, DPPH radical and hydroxyl radical. It was found that they inhibited CYP1A2 enzyme by uncompetitive inhibition. Apparent Ki values of CAF, EDPA, PEDPA, PMDPA and ODPA were 0.59, 0.39, 0.45, 0.75 and 0.80 µM, respectively suggesting potent inhibitors of CYP1A2. Moreover, they potentially scavenged nitric oxide radical with IC 50 values of 0.12, 0.22, 0.28, 0.22 and 0.51 mM, respectively. The IC50 values of superoxide anion scavenging were 0.20, 0.22, 0.44, 2.18 and 2.50 mM, respectively. 1, 1- diphenyl-2- picrylhydrazyl (DPPH) radical-scavenging ability, shown as IC50 values, were 0.41, 0.29, 0.30, 0.89 and 0.84 mM, respectively. Moreover, the hydroxyl radical scavenging in vitro model was shown as IC50 values of 23.22, 21.06, 17.10, 17.21 and 15.81 µM, respectively. From our results, caffeic acid and its amide analogues are in vitro inhibitors of human CYP1A2 catalytic activity and free radical formation. They may be useful to be developed as potential chemopreventive agents that block CYP1A2-mediated chemical carcinogenesis.

  7. Stabilization of Candida antarctica Lipase B (CALB Immobilized on Octyl Agarose by Treatment with Polyethyleneimine (PEI

    Directory of Open Access Journals (Sweden)

    Sara Peirce

    2016-06-01

    Full Text Available Lipase B from Candida antarctica (CALB was immobilized on octyl agarose (OC and physically modified with polyethyleneimine (PEI in order to confer a strong ion exchange character to the enzyme and thus enable the immobilization of other enzymes on its surface. The enzyme activity was fully maintained during the coating and the thermal stability was marginally improved. The enzyme release from the support by incubation in the non-ionic detergent Triton X-100 was more difficult after the PEI-coating, suggesting that some intermolecular physical crosslinking had occurred, making this desorption more difficult. Thermal stability was marginally improved, but the stability of the OCCALB-PEI was significantly better than that of OCCALB during inactivation in mixtures of aqueous buffer and organic cosolvents. SDS-PAGE analysis of the inactivated biocatalyst showed the OCCALB released some enzyme to the medium during inactivation, and this was partially prevented by coating with PEI. This effect was obtained without preventing the possibility of reuse of the support by incubation in 2% ionic detergents. That way, this modified CALB not only has a strong anion exchange nature, while maintaining the activity, but it also shows improved stability under diverse reaction conditions without affecting the reversibility of the immobilization.

  8. Selective sensing of mercury(II) using PVC-based membranes incorporating recently synthesized 1,3-alternate thiacalix[4]crown ionophore.

    Science.gov (United States)

    Mahajan, Rakesh Kumar; Kamal, Ajar; Kumar, Naresh; Bhalla, Vandana; Kumar, Manoj

    2013-05-01

    The construction and electrodes characteristics of poly(vinylchloride) (PVC)-based polymeric membrane electrode (PME) and coated graphite electrode (CGE), incorporating 1,3-alternate thiacalix[4]crown as ionophore for estimation of Hg(II) ions, are reported here. The best potential response was observed for PME-1 having membrane composition of: ionophore (6.2 mg), PVC (100.0 mg), 2-nitrophenyl octyl ether (2-NPOE; 200.0 mg), and sodium tetraphenyl borate (NaTPB; 2.0 mg); for CGE-1 with the membrane composition: ionophore (3.5 mg), PVC (40.0 mg), 2-NPOE (80.0 mg), and NaTPB (2.0 mg). The electrodes exhibits Nernstian slope of 29.16 mV/decade with PME-1 and 30.39 mV/decade with CGE-1 for Hg(II) ions over wide concentration range, i.e., 1.0 × 10(-1) to 5.0 × 10(-6) M with PME-1 and 1.0 × 10(-1) to 5.0 × 10(-7) M with CGE-1. Lower detection limits were found to be 9.77 × 10(-6) M for PME-1 and 7.76 × 10(-7) M for CGE-1 with response time varying from 10 to 20 s. Also, these electrodes work within pH range of 2.0-6.0 for PME-1 and 1.5-6.5 for CGE-1. Overall, CGE-1 has been found to be better than PME-1. CGE-1 has been used as indicator electrode for the potentiometric titration of Hg(II) ions with EDTA as well as successfully applied for determination of Hg(II) content in wastewater, insecticide, dental amalgam, and ayurvedic medicines samples with very good performance (0.9974 correlation coefficient in the comparison against volumetric method).

  9. In Vitro Bioavailability Study of an Antiviral Compound Enisamium Iodide

    OpenAIRE

    Eleonore Haltner-Ukomadu; Svitlana Gureyeva; Oleksii Burmaka; Andriy Goy; Lutz Mueller; Grygorii Kostyuk; Victor Margitich

    2018-01-01

    An investigation into the biopharmaceutics classification and a study of the in vitro bioavailability (permeability and solubility) of the antiviral compound enisamium iodide (4-(benzylcarbamoyl)-1-methylpyridinium iodide) were carried out. The solubility of enisamium iodide was determined in four different buffers. Apparent intestinal permeability (Papp) of enisamium iodide was assessed using human colon carcinoma (Caco-2) cells at three concentrations. The solubility of enisamium iodide in ...

  10. 2-[1-(1-Naphthyl-1H-1,2,3-triazol-4-yl]pyridine

    Directory of Open Access Journals (Sweden)

    Ulrich S. Schubert

    2009-05-01

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

  11. Structure and stability of the spinach aquaporin SoPIP2;1 in detergent micelles and lipid membranes.

    Directory of Open Access Journals (Sweden)

    Inés Plasencia

    Full Text Available BACKGROUND: SoPIP2;1 constitutes one of the major integral proteins in spinach leaf plasma membranes and belongs to the aquaporin family. SoPIP2;1 is a highly permeable and selective water channel that has been successfully overexpressed and purified with high yields. In order to optimize reconstitution of the purified protein into biomimetic systems, we have here for the first time characterized the structural stability of SoPIP2;1. METHODOLOGY/PRINCIPAL FINDING: We have characterized the protein structural stability after purification and after reconstitution into detergent micelles and proteoliposomes using circular dichroism and fluorescence spectroscopy techniques. The structure of SoPIP2;1 was analyzed either with the protein solubilized with octyl-β-D-glucopyranoside (OG or reconstituted into lipid membranes formed by E. coli lipids, diphytanoylphosphatidylcholine (DPhPC, or reconstituted into lipid membranes formed from mixtures of 1-palmitoyl-2-oleoyl-phosphatidylcholine (POPE, 1-palmitoyl-2oleoyl-phosphatidylethanolamine (POPE, 1-palmitoyl-2-oleoyl-phosphatidylserine (POPS, and ergosterol. Generally, SoPIP2;1 secondary structure was found to be predominantly α-helical in accordance with crystallographic data. The protein has a high thermal structural stability in detergent solutions, with an irreversible thermal unfolding occurring at a melting temperature of 58°C. Incorporation of the protein into lipid membranes increases the structural stability as evidenced by an increased melting temperature of up to 70°C. CONCLUSION/SIGNIFICANCE: The results of this study provide insights into SoPIP2;1 stability in various host membranes and suggest suitable choices of detergent and lipid composition for reconstitution of SoPIP2;1 into biomimetic membranes for biotechnological applications.

  12. Immobilized Lipases on Functionalized Silica Particles as Potential Biocatalysts for the Synthesis of  Fructose Oleate in an Organic Solvent/Water System

    OpenAIRE

    Vinicius Vescovi; Raquel L. C. Giordano; Adriano A. Mendes; Paulo W. Tardioli

    2017-01-01

    Lipases from Thermomyces lanuginosus (TLL) and Pseudomonas fluorescens (PFL) wereimmobilized on functionalized silica particles aiming their use in the synthesis of fructose oleate in a tert‐butyl alcohol/water system. Silica particles were chemically modified with octyl (OS), octyl plus glutaraldehyde (OSGlu), octyl plus glyoxyl(OSGlx), and octyl plus epoxy groups(OSEpx). PFL was hyperactivated on all functionalized supports (more than 100% recovered activity) using low protein loading (1 mg...

  13. Substitution Effects and Linear Free Energy Relationships During Reduction of 4- Benzoyl-n-(4-substituted Benzyl)pyridinium Cations

    Science.gov (United States)

    Leventis, Nicholas; Zhang, Guo-Hui; Rawashdeh, Abdel-Monem M.; Sotiriou-Leventis, Chariklia; Gray, Hugh R. (Technical Monitor)

    2003-01-01

    In analogy to 4-(para-substituted benzoyl)-N-methylpyridinium cations (1-X's), the title species (2-X's, -X = -OCH3, -CH3, -H, -Br, -COCH3, -NO2) undergo two reversible, well-separated (E(sub 1/2) greater than or equal to 650 mV) one-electron reductions. The effect of substitution on the reduction potentials of 2-X's is much weaker than the effect of the same substituents on 1-X's: the Hammett rho-values are 0.80 and 0.93 for the 1st- and 2nd-e reduction of 2-X's vs. 2.3 and 3.3 for the same reductions of 1-X's, respectively. Importantly, the nitro group of 2-NO2 undergoes reduction before the 2nd-e reduction of the 4-benzoylpyridinium system. These results suggest that the redox potentials of the 4-benzoylpyridinium system can be course-tuned via p-benzoyl substitution and fine-tuned via para-benzyl substitution. Introducing the recently derived substituent constant of the -NO2(sup)- group (sigma para-NO2(sup)- = -0.97) yields an excellent correlation for the 3rd-e reduction of 2- NO2 (corresponding to the reduction of the carbonyl group) with the 2nd-e reduction of the other 2-X's, and confirms the electron donating properties of -NO2(sup)-.

  14. Volatile Constituents of Different Plant Parts and Populations of Malabaila aurea Boiss. from Montenegro

    Directory of Open Access Journals (Sweden)

    Ivan Vučković

    2014-03-01

    Full Text Available The volatile constituents of different plant parts and populations of Malabaila aurea Boiss. from Montenegro were obtained by simultaneous distillation-extraction and analyzed by GC-FID and GC-MS. A total of 12 samples were examined and 45 compounds were identified. The volatile content of different M. aurea populations was very similar, while the volatile fractions obtained from different plant parts showed significant qualitative and quantitative differences. The most abundant compounds found in stems & leaves were apiole (51.0-56.3%, myristicin (16.3-25.4%, and falcarinol (4.1-10.7%. The roots showed the same major components, but with different relative abundances: 30.9-49.1% of apiole, 12.9-34.7% of falcarinol, and 9.9-31.1% of myristicin. The volatile constituents of fruits & flowers were remarkably different, containing up to 71.2-80.5% octyl butyrate, 11.4-18.0% octanol, and 2.7-6.8% octyl hexanoate. The results were discussed as possible indication of relatedness of Malabaila aurea and Pastinacasativa (parsnip .

  15. 1,4-Disilacyclohexa-2,5-diene

    DEFF Research Database (Denmark)

    Tibbelin, Julius; Wallner, Andreas; Emanuelsson, Rikard

    2014-01-01

    2,3,5,6-Tetraethyl-1,4-disilacyclohexa-2,5-dienes with either four chloro (1a), methyl (1b), or trimethylsilyl (TMS) (1c) substituents at the two silicon atoms were examined in an effort to design rigid compounds with strong neutral cross-hyperconjugation between π- and σ-bonded molecular segments......). Furthermore, 1,4-disilacyclohexadiene 1c absorbs strongly at 273 nm (4.55 eV), whereas 1a and 1b have no symmetry allowed excitations above 215 nm (below 5.77 eV). Thus, suitably substituted 1,4-disilacyclohexa-2,5-dienes could represent novel building blocks for the design of larger cross...

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

    Directory of Open Access Journals (Sweden)

    Dongamanti Ashok

    2015-06-01

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

  17. Are 1,4- and 1,5-disubstituted 1,2,3-triazoles good pharmacophoric groups?

    Science.gov (United States)

    Massarotti, Alberto; Aprile, Silvio; Mercalli, Valentina; Del Grosso, Erika; Grosa, Giorgio; Sorba, Giovanni; Tron, Gian Cesare

    2014-11-01

    Over the last decade, 1,2,3-triazoles have received increasing attention in medicinal chemistry thanks to the discovery of the highly useful and widely applicable 1,3-dipolar cycloaddition reaction between azides and alkynes (click chemistry) catalyzed by copper salts and ruthenium complexes. After a decade of medicinal chemistry research on 1,2,3-triazoles, we feel that the time is ripe to demonstrate the real ability of this heterocycle to participate in important and pivotal binding interactions with biological targets while maintaining a good pharmacokinetic profile. In this study, we retrieved and analyzed X-ray crystal structures of complexes between 1,2,3-triazoles and either proteins or DNA to understand the pharmacophoric role of the triazole. Furthermore, the metabolic stability, the capacity to inhibit cytochromes, and the contribution of 1,2,3-triazoles to the overall aqueous solubility of compounds containing them have been analyzed. This information should furnish fresh insight for medicinal chemists in the design of novel bioactive molecules that contain the triazole nucleus. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. The B(E2;4^+1->2^+1) / B(E2;2^+1->0^+1) Ratio in Even-Even Nuclei

    Science.gov (United States)

    Loelius, C.; Sharon, Y. Y.; Zamick, L.; G"Urdal, G.

    2009-10-01

    We considered 207 even-even nuclei throughout the chart of nuclides for which the NNDC Tables had data on the energies and lifetimes of the 2^+1 and 4^+1 states. Using these data we calculated for each nucleus the electric quadrupole transition strengths B(E2;4^+1->2^+1) and B(E2;2^+1->0^+1), as well as their ratio. The internal conversion coefficients were obtained by using the NNDC HSICC calculator. For each nucleus we plotted the B(E2) ratio against A, N, and Z. We found that for close to 90% of the nuclei considered the ratio had values between 0.5 and 2.5. Most of the outliers had magic numbers of protons or neutrons. Our ratio results were compared with the theoretical predictions for this ratio by different models--10/7 in the rotational model and 2 in the simplest vibrational model. In the rotational regions (for 150 220) the ratios were indeed close to 10/7. For the few nuclei thought to be vibrational the ratios were usually less than 2. Otherwise, we got a wide scatter of ratio values. Hence other models, including the NpNn scheme, must be considered in interpreting these results.

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

    International Nuclear Information System (INIS)

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

    1985-01-01

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

  20. Residues of 2, 4-D in air samples from Saskatchewan: 1966-1975.

    Science.gov (United States)

    Grover, R; Kerr, L A; Wallace, K; Yoshida, K; Maybank, J

    1976-01-01

    Residues of 2,4-D (2,4-dichlorophenoxyacetic acid) in air samples from several sampling sites in central and southern Saskatchewan during the spraying seasons in the 1966-68 and 1970-75 periods were determined by gas-liquid chromatographic techniques. Initially, individual esters of 2,4-D were characterized by retention times and confirmed further by co-injection and dual column procedures. Since 1973, however, only total 2,4-D acid levels in air samples have been determined after esterification to the methyl ester and confirmed by gc/ms techniques whenever possible. Up to 50% of the daily samples collected during the spraying season at any of the locations and during any given year contained 2,4-D, with butyl esters being found most frequently. The daily 24-hr mean atmospheric concentrations of 2,4-D ranged from 0.01 to 1.22 mug/m3, 0.01 to 13.50 mug/m3, and 0.05 to 0.59 mug/m3 for the iso-propyl, mixed butyl and iso-octyl esters, respectively. Even when the samples were analysed for the total 2,4-D content, i.e. from 1973 onwards, the maximum level of the total acid reached only 23.14 mug/m3. In any given year and at any of the sampling sites, about 30% of the samples contained less than 0.01 mug/m3 of 2,4-D. In another 40% of the samples, the levels of 2,4-D ranged from 0.01 to 0.099 mug/m3. Only about 30% of the samples contained 2,4-D concentrations higher than 0.1 mug/m3, with only 10% or less exceeding 1 mug/m3. None of the samples, obtained with the high volume particulate sampler, showed any detectable levels of 2,4-D, indicating little or no transport of 2,4-D adsorbed on dust particles or as crystals of amine salts.

  1. Crystal structures of three co-crystals of 1,2-bis-(pyridin-4-yl)ethane with 4-alk-oxy-benzoic acids: 4-eth-oxy-benzoic acid-1,2-bis-(pyridin-4-yl)ethane (2/1), 4-n-propoxybenzoic acid-1,2-bis(pyridin-4-yl)ethane (2/1) and 4-n-but-oxy-benzoic acid-1,2-bis-(pyridin-4-yl)ethane (2/1).

    Science.gov (United States)

    Tabuchi, Yohei; Gotoh, Kazuma; Ishida, Hiroyuki

    2015-11-01

    The crystal structures of three hydrogen-bonded co-crystals of 4-alk-oxy-benzoic acid-1,2-bis-(pyridin-4-yl)ethane (2/1), namely, 2C9H10O3·C12H12N2, (I), 2C10H12O3·C12H12N2, (II), and 2C11H14O3·C12H12N2, (III), have been determined at 93, 290 and 93 K, respectively. In (I), the asymmetric unit consists of one 4-eth-oxy-benzoic acid mol-ecule and one half-mol-ecule of 1,2-bis-(pyridin-4-yl)ethane, which lies on an inversion centre. In (II) and (III), the asymmetric units each comprise two crystallographically independent 4-alk-oxy-benzoic acid mol-ecules and one 1,2-bis-(pyridin-4-yl)ethane mol-ecule. In each crystal, the two components are linked by O-H⋯N hydrogen bonds, forming a linear hydrogen-bonded 2:1unit of the acid and the base. Similar to the structure of 2:1 unit of (I), the units of (II) and (III) adopt nearly pseudo-inversion symmetry. The 2:1 units of (I), (II) and (III) are linked via C-H⋯O hydrogen bonds, forming tape structures.

  2. Crystal structures of pure 3-(4-bromo-2-chlorophenyl-1-(pyridin-4-ylbenzo[4,5]imidazo[1,2-d][1,2,4]triazin-4(3H-one and contaminated with 3-(4-bromophenyl-1-(pyridin-4-ylbenzo[4,5]imidazo[1,2-d][1,2,4]triazin-4(3H-one

    Directory of Open Access Journals (Sweden)

    Kanan Wahedy

    2017-09-01

    Full Text Available The side product of the cyclocondensation reaction between ethyl benzimidazole-2-carboxylate and the nitrile imine of the corresponding hydrazonyl chloride, C20H11BrClN5O, crystallized in two crystal forms. Form (1 is a co-crystal of the target compound (without any chlorine substituent and a side product containing a Cl atom in position 2 of the bromophenyl group, C20H12BrN5O·0.143C20H11BrClN5O. (2 contains the pure side product. The slightly different conformation of the ring systems leads to a different packing of (1 and (2, but both crystal structures are dominated by π–π interactions.

  3. Osmotic coefficients of binary mixtures of four ionic liquids with ethanol or water at T = (313.15 and 333.15) K

    International Nuclear Information System (INIS)

    Calvar, Noelia; Gonzalez, Begona; Dominguez, Angeles; Macedo, Eugenia A.

    2009-01-01

    Measurements of osmotic coefficients of BmimCl (1-butyl-3-methylimidazolium chloride) and HmimCl (1-hexyl-3-methylimidazolium chloride) with ethanol and EmimEtSO 4 (1-ethyl-3-methylimidazolium ethylsulfate) and EmpyEtSO 4 (1-ethyl-3-methylpyridinium ethylsulfate) with water at T = (313.15 and 333.15) K are reported in this work. Vapour pressure and activity results of the studied binary systems are obtained from experimental measurements. The results for the osmotic coefficients are correlated using the extended Pitzer model modified by Archer and the modified NRTL (MNRTL) model. The standard deviations obtained with both models are also given. The parameters obtained with the extended Pitzer model of Archer are used to calculate the mean molal activity coefficients

  4. Sigma-1 receptor agonists directly inhibit Nav1.2/1.4 channels.

    Directory of Open Access Journals (Sweden)

    Xiao-Fei Gao

    Full Text Available (+-SKF 10047 (N-allyl-normetazocine is a prototypic and specific sigma-1 receptor agonist that has been used extensively to study the function of sigma-1 receptors. (+-SKF 10047 inhibits K(+, Na(+ and Ca2+ channels via sigma-1 receptor activation. We found that (+-SKF 10047 inhibited Na(V1.2 and Na(V1.4 channels independently of sigma-1 receptor activation. (+-SKF 10047 equally inhibited Na(V1.2/1.4 channel currents in HEK293T cells with abundant sigma-1 receptor expression and in COS-7 cells, which barely express sigma-1 receptors. The sigma-1 receptor antagonists BD 1063,BD 1047 and NE-100 did not block the inhibitory effects of (+-SKF-10047. Blocking of the PKA, PKC and G-protein pathways did not affect (+-SKF 10047 inhibition of Na(V1.2 channel currents. The sigma-1 receptor agonists Dextromethorphan (DM and 1,3-di-o-tolyl-guanidine (DTG also inhibited Na(V1.2 currents through a sigma-1 receptor-independent pathway. The (+-SKF 10047 inhibition of Na(V1.2 currents was use- and frequency-dependent. Point mutations demonstrated the importance of Phe(1764 and Tyr(1771 in the IV-segment 6 domain of the Na(V1.2 channel and Phe(1579 in the Na(V1.4 channel for (+-SKF 10047 inhibition. In conclusion, our results suggest that sigma-1 receptor agonists directly inhibit Na(V1.2/1.4 channels and that these interactions should be given special attention for future sigma-1 receptor function studies.

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

    Science.gov (United States)

    Rao, Guo-Wu; Hu, Wei-Xiao

    2003-05-01

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

  6. Crystal structure of tetrabutylammonium bromide–1,2-diiodo-3,4,5,6-tetrafluorobenzene–dichloromethane (2/2/1

    Directory of Open Access Journals (Sweden)

    Jasmine Viger-Gravel

    2015-05-01

    Full Text Available The crystallization of a 1:1 molar solution of 1,2-diiodo-3,4,5,6-tetrafluorobenzene (o-DITFB and tetrabutylammonium bromide (n-Bu4NBr from dichloromethane yielded pure white crystals of a halogen-bonded compound, C16H36N+·Br−·C6F4I2·0.5CH2Cl2 or [(n-Bu4NBr(o-DITFB]·0.5CH2Cl2. The compound may be described as a quaternary system and may be classified as a salt–cocrystal solvate. The asymmetric unit contains one molecule of solvent, two o-DITFB molecules, two cations (n-Bu4N+ and two crystallographically distinct bromide ions [θI...Br-...I = 144.18 (1 and 135.35 (1°]. The bromide ion is a bidentate halogen-bond acceptor which interacts with two covalently bonded iodines (i.e. halogen-bond donors, resulting in a one-dimensional polymeric zigzag chain network approximately along the a axis. The observed short contacts and angles are characteristic of the non-covalent interaction [dC—I...Br = 3.1593 (4–3.2590 (5 Å; θC—I...Br = 174.89 (7 and 178.16 (7°]. It is noted that iodine acts as both a halogen-bond donor and a weak CH hydrogen-bond acceptor, while the bromide ions act as acceptors for weak CH hydrogen bonds and halogen bonds.

  7. Crystal structures of the 2:2 complex of 1,1′-(1,2-phenylenebis(3-m-tolylurea and tetrabutylammonium chloride or bromide

    Directory of Open Access Journals (Sweden)

    Chao Huang

    2017-09-01

    Full Text Available The title compounds, tetrabutylammonium chloride–1,1′-(1,2-phenylenebis(3-m-tolylurea (1/1, C16H36N+·Cl−·C22H22N4O2 or [(n-Bu4N+·Cl−(C22H22N4O2] (I and tetrabutylammonium bromide–1,1′-(1,2-phenylenebis(3-m-tolylurea (1/1, C16H36N+·Br−·C22H22N4O2 or [(n-Bu4N+·Br−(C22H22N4O2] (II, both comprise a tetrabutylammonium cation, a halide anion and an ortho-phenylene bis-urea molecule. Each halide ion shows four N—H...X (X = Cl or Br interactions with two urea receptor sites of different bis-urea moieties. A crystallographic inversion centre leads to the formation of a 2:2 arrangement of two halide anions and two bis-urea molecules. In the crystals, the dihedral angle between the two urea groups of the bis-urea molecule in (I [defined by the four N atoms, 165.4 (2°] is slightly smaller than that in (II [167.4 (2°], which is probably due to the smaller ionic radius of chloride compared to bromide.

  8. Synthesis and antimicrobial activity of chromone-linked 2-pyridone fused with 1,2,4-triazoles, 1,2,4-triazines and 1,2,4-triazepines ring systems

    International Nuclear Information System (INIS)

    Ali, Tarik El-Sayed; Ibrahim, Magdy Ahmed

    2010-01-01

    Three series of novel fused nitrogen heterocyclic systems such as 1,2,4-triazolo[1,5-a ] pyridines (5-7 and 9), pyrido[1,2-b][1,2,4]triazines (10, 11, 13 and 15), and pyrido[1,2-b][1,2,4]triazepines (17, 18, 20 and 22) linked with a chromone moiety were synthesized from the key intermediate 1,6-diamino-(6-chloro-4-oxo-4H-chromen-3-yl)-2-oxo-1,2-dihydropyridine-3,5- dicarbonitrile (4) with some electrophilic reagents. The structures of the novel compounds were established by elemental analyses and spectral data. All the products were also screened in vitro for their antimicrobial activity. Compounds 7, 9 and 15 showed the highest activities when compared with the reference drugs. (author)

  9. Photomagnetic studies on spin-crossover solid solutions containing two different metal complexes, [Fe(1-bpp)(2)](x)[M(terpy)2](1-x)[BF4]2 (M = Ru or Co).

    Science.gov (United States)

    Chastanet, Guillaume; Tovee, Clare A; Hyett, Geoffrey; Halcrow, Malcolm A; Létard, Jean-François

    2012-04-28

    The photomagnetic properties of two series of spin-crossover solid solutions, [Fe(1-bpp)(2)](x)[Ru(terpy)(2)](1-x)(BF(4))(2) and [Fe(1-bpp)(2)](x)[Co(terpy)(2)](1-x)(BF(4))(2) (1-bpp = 2,6-bis[pyrazol-1-yl]pyridine), have been investigated. For all the materials, the evolution of the T(LIESST) value, the high-spin → low-spin relaxation parameters and the LITH loops were thoroughly studied. Interestingly in the Fe:Co series, along the photo-excitation, cobalt ions are concomitantly converted from low-spin to high-spin states with the iron centres, and also fully relax after light excitation. This journal is © The Royal Society of Chemistry 2012

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  11. Synthesis of new 1H-1,2,3-triazole-1,4-naphthoquinones

    Directory of Open Access Journals (Sweden)

    Wagner O. Valença

    2012-06-01

    Full Text Available In this work, were synthesized new 1H-1,2,3-triazole-1,4-naphthoquinones via 1,3-dipolar cycloaddition reaction using CuI/acetonitrile without addition of base or ligand. The compounds (3a-i were obtained in moderate-to-good yields 45-92%. To prepare (3d, we obtain a mixture of (3d and (4 in a ratio 3:1, that it was difficult to separate. The low yield for the compound (3f can be also justified based in the formation of aminonaphthoquinone (4. The acetylation of (3h and (3i afforded the compounds (5 and (6 in 77% and 35% of yields, respectively. The low yield of (6 was due to formation of 35 % of the elimination product (7.

  12. New open-framework three-dimensional lanthanide oxalates containing as a template the diprotonated 1,2- or 1,3-diaminopropane

    International Nuclear Information System (INIS)

    Mohanu, A.; Brouca-Cabarrecq, C.; Trombe, J.C.

    2006-01-01

    Single crystals of three new open-framework lanthanide oxalates have been synthesized hydrothermally, in the presence of 1,2-diaminopropane, (C 3 N 2 H 12 )[Nd(H 2 O)(C 2 O 4 ) 2 ] 2 .3H 2 O I and (C 3 N 2 H 12 )[Yb(C 2 O 4 ) 2 ] 2 .5H 2 O II, or 1,3-diaminopropane (C 3 N 2 H 12 ) 2 [La 2 (C 2 O 4 ) 5 ].5H 2 O III. Their structures have been determined by X-ray diffraction data: I and III crystallize in the triclinic system, space group P-1, with a=7.8130(5)A, b=11.8800(6)A, c=12.9940(8)A, α=93.092(5) o , β=93.930(6) o , γ=108.359(5) o and a=11.6650(9)A, b=11.9240(6)A, c=13.2230(7)A, α=104.585(4) o , β=108.268(5) o , γ=111.132(5) o , respectively while II crystallizes in the orthorhombic system, space group F2dd, with a=8.7970(4)A, b=16.1550(8)A, c=32.170(2)A. The three-dimensional (3D) framework of these compounds is built up by the linkages of lanthanide atoms and the oxygen atoms of the bischelating oxalate ligands. Instead of four chelating oxalate units surrounding a lanthanide atom (I and II), both lanthanum atoms, in III, are surrounded by five chelating oxalate groups and that is new. In all the cases within the frame, are observed 8- and 12-membered channels where are localized the guest species, 1,2- or 1,3-diaminopropane cations and free water molecules. The ratio of the guest number (especially the diaminopropane) per 12-membered ring could tune the shape and the size of 12-membered channels: thus, the 12-membered channels, observed for I and II, have elliptical cross-section (5.5Ax11.4A and 5.2Ax9.5A) while those, observed for III, have nearly circular cross-section (9.1Ax9.5A). The lanthanide atoms are 8, 9 and 10-fold coordinated for Yb (II), Nd (I) and La (III), respectively

  13. CERES ERBE-like Monthly Geographical Averages (ES-4) in HDF (CER_ES4_FM1+FM2_Edition1)

    Science.gov (United States)

    Wielicki, Bruce A. (Principal Investigator)

    The ERBE-like Monthly Geographical Averages (ES-4) product contains a month of space and time averaged Clouds and the Earth's Radiant Energy System (CERES) data for a single scanner instrument. The ES-4 is also produced for combinations of scanner instruments. For each observed 2.5-degree spatial region, the daily average, the hourly average over the month, and the overall monthly average of shortwave and longwave fluxes at the Top-of-the-Atmosphere (TOA) from the CERES ES-9 product are spatially nested up from 2.5-degree regions to 5- and 10-degree regions, to 2.5-, 5-, and 10-degree zonal averages, and to global monthly averages. For each nested area, the albedo and net flux are given. For each region, the daily average flux is estimated from an algorithm that uses the available hourly data, scene identification data, and diurnal models. This algorithm is 'like' the algorithm used for the Earth Radiation Budget Experiment (ERBE). The following CERES ES4 data sets are currently available: CER_ES4_FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition2 CER_ES4_PFM+FM1_Edition1 CER_ES4_PFM+FM2_Edition1 CER_ES4_TRMM-PFM_Edition1 CER_ES4_TRMM-PFM_Edition2 CER_ES4_Terra-FM1_Edition1 CER_ES4_Terra-FM2_Edition1 CER_ES4_FM1+FM2_Edition2 CER_ES4_Terra-FM1_Edition2 CER_ES4_Terra-FM2_Edition2 CER_ES4_Aqua-FM3_Edition1 CER_ES4_Aqua-FM4_Edition1 CER_ES4_FM1+FM2+FM3+FM4_Edition1 CER_ES4_Aqua-FM3_Edition2 CER_ES4_Aqua-FM4_Edition2 CER_ES4_FM1+FM3_Edition2 CER_ES4_FM1+FM4_Edition2 CER_ES4_PFM+FM1_Edition2 CER_ES4_PFM+FM2_Edition2 CER_ES4_Aqua-FM3_Edition1-CV CER_ES4_Aqua-FM4_Edition1-CV CER_ES4_Terra-FM1_Edition1-CV CER_ES4_Terra-FM2_Edition1-CV. [Location=GLOBAL] [Temporal_Coverage: Start_Date=1998-01-01; Stop_Date=2003-12-31] [Spatial_Coverage: Southernmost_Latitude=-90; Northernmost_Latitude=90; Westernmost_Longitude=-180; Easternmost_Longitude=180] [Data_Resolution: Latitude_Resolution=2.5 degree; Longitude_Resolution=2.5 degree; Horizontal

  14. Purification of neuraminidase from Influenza virus subtype H5N1

    Directory of Open Access Journals (Sweden)

    Simson Tariga

    2009-03-01

    Full Text Available Influenza-virus neuraminidase plays vital role in the survival of the organisms. Vaccination of animals with this glycoprotein confers immune responses so that enable it to protect the animals from incoming infection. Supplementation of conventional vaccines with this glycoprotein increases the protection and longevity of the vaccine. Purified neuraminidase can also be used to develop serological tests for differentiation of serologically positive animals due to infection or to vaccination. In this study purification of neuraminidase from influenza virus subtype H5N1 was described. Triton x-100 and Octyl β-D-glucopyranoside were used to extract and diluted the glycoprotein membrane. The enzymatic activity of the neuraminidase was assayed using a fluorochrome substrate, 4-methylumbelliferyl-a-D-N-acetyl neuraminic acid, which was found to be simple, sensitive and suitable for the purification purpose. The neuraminidase was absorbed selectively on an oxamic-acid agarose column. The purity of neuraminidase eluted from this affinity column was high. A higher purity of the neuraminidase was obtained by further separation with gel filtration on Superdex-200. The purified neuraminidase was enzymatically active and did not contain any detectable haemagglutinin, either by haemagglutination assay or by monospecific antibodies raised against H5N1 hemagglutinin. The purified neuraminidase was recognized strongly by antibodies raised against an internal but only weakly by that against C-terminal regions of the neuraminidase protein of H5N1-influenza virus. The purified neuraminidase was in tetrameric forms but dissociated into monomeric form on reducing condition, or mostly dimeric form on non-reducing SDS-PAGE.

  15. DFT, spectroscopic studies, NBO, NLO and Fukui functional analysis of 1-(1-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethylidene) thiosemicarbazide

    Science.gov (United States)

    Zacharias, Adway Ouseph; Varghese, Anitha; Akshaya, K. B.; Savitha, M. S.; George, Louis

    2018-04-01

    A novel triazole derivative 1-(1-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethylidene) thiosemicarbazide was synthesized and subjected to density functional theory (DFT) studies employing B3LYP/6-31+G(d,p) basis set. Characterization was done by FT-IR, Raman, mass, 1H NMR and 13C NMR spectroscopic analyses. The stability of the molecule was evaluated from NBO studies. Delocalization of electron charge density and hyper-conjugative interactions were accountable for the stability of the molecule. The dipole moment (μ), mean polarizabilty (△α) and first order hyperpolarizability (β) of the molecule were calculated. Molecular electrostatic potential studies, HOMO-LUMO and thermodynamic properties were also determined. HOMO and LUMO energies were experimentally determined by Cyclic Voltammetry.

  16. 2,2′-{1,1′-[Butane-1,4-diylbis(oxynitrilo]diethylidyne}di-1-naphthol

    Directory of Open Access Journals (Sweden)

    Wen-Kui Dong

    2009-06-01

    Full Text Available The title compound, C28H28N2O4, was synthesized by the reaction of 2-acetyl-1-naphthol with 1,4-bis(aminooxybutane in ethanol. The molecule, which lies about an inversion centre, adopts a linear structure, in which the oxime groups and naphthalene ring systems assume an anti conformation. The intramolecular interplanar distance between parallel naphthalene rings is 1.054 (3 Å. Intramolecular O—H...N hydrogen bonds are formed between the oxime nitrogen and hydroxy groups.

  17. In Situ Electrochemical SFG/DFG Study of CN and Nitrile Adsorption at Au from 1-Butyl-1-methyl-pyrrolidinium Bis(trifluoromethylsulfonyl Amide Ionic Liquid ([BMP][TFSA] Containing 4-{2-[1-(2-Cyanoethyl-1,2,3,4-tetrahydroquinolin-6-yl]diazenyl} Benzonitrile (CTDB and K[Au(CN2

    Directory of Open Access Journals (Sweden)

    Benedetto Bozzini

    2012-06-01

    Full Text Available In this paper we report an in situ electrochemical Sum-/Difference Frequency Generation (SFG/DFG spectroscopy investigation of the adsorption of nitrile and CN from the ionic liquid 1-butyl-1-methyl-pyrrolidinium bis(trifluoromethylsulfonyl amide ([BMP][TFSA] containing 4-{2-[1-(2-cyanoethyl-1,2,3,4-tetrahydroquinolin-6-yl]- diazenyl}benzonitrile (CTDB at Au electrodes in the absence and in the presence of the Au-electrodeposition process from K[Au(CN2]. The adsorption of nitrile and its coadsorption with CN resulting either from the cathodic decomposition of the dye or from ligand release from the Au(I cyanocomplex yield potential-dependent single or double SFG bands in the range 2,125–2,140 cm1, exhibiting Stark tuning values of ca. 3 and 1 cm1 V1 in the absence and presence of electrodeposition, respectively. The low Stark tuning found during electrodeposition correlates with the cathodic inhibiting effect of CTDB, giving rise to its levelling properties. The essential insensitivity of the other DFG parameters to the electrodeposition process is due to the growth of smooth Au.

  18. Metabolism of 1-fluoro-1,1,2-trichloroethane, 1,2-dichloro-1,1-difluoroethane, and 1,1,1-trifluoro-2-chloroethane.

    Science.gov (United States)

    Yin, H; Jones, J P; Anders, M W

    1995-03-01

    1-Fluoro-1,1,2-trichloroethane (HCFC-131a), 1,2-dichloro-1,1-difluoroethane (HCFC-132b), and 1,1,1-trifluoro-2-chloroethane (HCFC-133a) were chosen as models for comparative metabolism studies on 1,1,1,2-tetrahaloethanes, which are under consideration as replacements for ozone-depleting chlorofluorocarbons (CFCs). Male Fischer 344 rats were given 10 mmol/kg ip HCFC-131a or HCFC-132b or exposed by inhalation to 1% HCFC-133a for 2 h. Urine collected in the first 24 h after exposure was analyzed by 19F NMR and GC/MS and with a fluoride-selective ion electrode for the formation of fluorine-containing metabolites. Metabolites of HCFC-131a included 2,2-dichloro-2-fluoroethyl glucuronide, 2,2-dichloro-2-fluoroethyl sulfate, dichlorofluoroacetic acid, and inorganic fluoride. Metabolites of HCFC-132b were characterized as 2-chloro-2,2-difluoroethyl glucuronide, 2-chloro-2,2-difluoroethyl sulfate, chlorodifluoroacetic acid, chlorodifluoroacetaldehyde hydrate, chlorodifluoroacetaldehyde-urea adduct, and inorganic fluoride. HCFC-133a was metabolized to 2,2,2-trifluoroethyl glucuronide, trifluoroacetic acid, trifluoroacetaldehyde hydrate, trifluoroacetaldehyde-urea adduct, inorganic fluoride, and a minor, unidentified metabolite. With HCFC-131a and HCFC-132b, glucuronide conjugates of 2,2,2-trihaloethanols were the major urinary metabolites, whereas with HCFC-133a, a trifluoroacetaldehyde-urea adduct was the major urinary metabolite. Analysis of metabolite distribution in vivo indicated that aldehydic metabolites increased as fluorine substitution increased in the order HCFC-131a < HCFC-132b < HCFC-133a. With NADPH-fortified rat liver microsomes, HCFC-133a and HCFC-132b were biotransformed to trifluoroacetaldehyde and chlorodifluoroacetaldehyde, respectively, whereas HCFC-131a was converted to dichlorofluoroacetic acid. No covalently bound metabolites were detected by 19F NMR spectroscopy.(ABSTRACT TRUNCATED AT 250 WORDS)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Ming-qiang Qiu

    2010-08-01

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

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

    Directory of Open Access Journals (Sweden)

    V. I. Pavlovsky

    2014-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1982-01-01

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

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

    Science.gov (United States)

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

    2014-10-17

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

  4. Extraction of Am(III) using novel solvent systems containing a tripodal diglycolamide ligand in room temperature ionic liquids: a 'green' approach for radioactive waste processing

    NARCIS (Netherlands)

    Sengupta, A; Mohapatra, P.K.; Iqbal, M.; Verboom, Willem; Huskens, Jurriaan; Godbole, S.V.

    2012-01-01

    Extraction of Am3+ from acidic feed solutions was investigated using novel solvent systems containing a tripodal diglycolamide (T-DGA) in three room temperature ionic liquids (RTIL), viz. [C4mim][NTf2], [C6mim][NTf2] and [C8mim][NTf2]. Compared to the results obtained with N,N,N′,N′-tetra-n-octyl

  5. Effect of alkyl chain length on the rotational diffusion of nonpolar and ionic solutes in 1-alkyl-3-methylimidazolium-bis(trifluoromethylsulfonyl)imides.

    Science.gov (United States)

    Gangamallaiah, V; Dutt, G B

    2013-10-10

    Rotational diffusion of a nonpolar solute 9-phenylanthracene (9-PA) and a cationic solute rhodamine 110 (R110) has been examined in a series of 1-alkyl-3-methylimidazolium (alkyl = octyl, decyl, dodecyl, tetradecyl, hexadecyl, and octadecyl) bis(trifluoromethylsulfonyl)imides to understand the influence of alkyl chain length on solute rotation. In this study, reorientation times (τr) have been measured as a function of viscosity (η) by varying the temperature (T) of the solvents. These results have been analyzed using the Stokes-Einstein-Debye (SED) hydrodynamic theory along with the ones obtained for the same solutes in 1-alkyl-3-methylimidazolium (alkyl = methyl, ethyl, propyl, butyl, and hexyl) bis(trifluoromethylsulfonyl)imides (Gangamallaiah and Dutt, J. Phys. Chem. B 2012, 116, 12819-12825). It has been noticed that the data for 9-PA and R110 follows the relation τr = A(η/T)(n) with A being the ratio of hydrodynamic volume of the solute to the Boltzmann constant and n = 1 as envisaged by the SED theory. However, upon increasing the alkyl chain length from methyl to octadecyl significant deviations from the SED theory have been observed especially from the octyl derivative onward. From methyl to octadecyl derivatives, the value of A decreases by a factor of 3 for both the solutes and n by a factor of 1.4 and 1.6 for 9-PA and R110, respectively. These observations have been rationalized by taking into consideration the organized structure of the ionic liquids, whose influence appears to be pronounced when the number of carbon atoms in the alkyl chain attached to the imidazolium cation exceeds eight.

  6. 1-[3-(2-Methyl-4-phenylquinolin-3-yl-5-phenyl-4,5-dihydro-1H-pyrazol-1-yl]-propane-1-one

    Directory of Open Access Journals (Sweden)

    Allaoua Kedjadja

    2015-06-01

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

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

    Directory of Open Access Journals (Sweden)

    Mohamed G. Marei

    2011-12-01

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

  8. Record high-nuclearity polyoxoniobates. Discrete nanoclusters {Nb_1_1_4}, {Nb_8_1}, and {Nb_5_2}, and extended frameworks based on {Cu_3Nb_7_8} and {Cu_4Nb_7_8}

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Lu; Zhu, Zeng-Kui; Wu, Yan-Lan; Qi, Yan-Jie; Li, Xin-Xiong; Zheng, Shou-Tian [State Key Laboratory of Photocatalysis on Energy and Environment, College of Chemistry, Fuzhou University, Fujian (China)

    2017-12-18

    A series containing the highest nuclearity polyoxoniobate (PONb) nanoclusters, ranging from dimers to tetramers, has been obtained. They include one 114-nuclear {Li_8 is contained in Nb_1_1_4O_3_1_6}, one 81-nuclear {Li_3K is contained in Nb_8_1O_2_2_5}, and one 52-nuclear {H_4Nb_5_2O_1_5_0}. The Nb nuclearity of these PONbs is remarkably larger than those of all known high-nuclearity PONbs (≤32). Furthermore, the introduction of 3d Cu{sup 2+} ions can lead to the generation of extended inorganic-organic hybrid frameworks built from novel, high-nuclearity, nanoscale heterometallic PONb building blocks {H_3Cu_3Nb_7_8O_2_2_2} or {H_3Cu_4(en)Nb_7_8O_2_2_2}. These building blocks also contain the largest number of Nb centers of any heterometallic PONbs reported to date. The synthesis of new-type PONbs has long been a challenging subject in PONb chemistry. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Synthesis of dimethyl-1,1 guanylguanidine-{sup 14}C-2,4 (dimethyl-1-1 biguanide) hydrochloride; Synthese du chlorhydrate de dimethyl-1,1 guanylguanidine {sup 14}C-2,4 (dimethyl-1-1 biguanide)

    Energy Technology Data Exchange (ETDEWEB)

    Herbert, M; Pichat, L [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1961-07-01

    A description of the synthesis of dimethyl-1,1 guanylguanidine-{sup 14}C-2,4 hydrochloride passing through the {sup 14}C{sub 2} dicyandiamide. The overall yield with respect to Ba{sup 14}CO{sub 3} is 38 per cent. (author) [French] Description de la synthese du chlorhydrate de dimethyl-1,1 guanylguanidine {sup 14}C-2,4 par l'intermediaire de la dicyandiamide {sup 14}C{sub 2}. Le rendement global par rapport a {sup 14}CO{sub 3}Ba est de 38 pour cent. (auteur)

  10. Biodegradation of 1,1,1-trichloro-2,2-bis(4-chlorophenyl) ethane (DDT) by using Serratia marcescens NCIM 2919.

    Science.gov (United States)

    Grewal, Jasneet; Bhattacharya, Amrik; Kumar, Sumit; Singh, Dileep K; Khare, Sunil K

    2016-12-01

    A solvent tolerant bacterium Serratia marcescens NCIM 2919 has been evaluated for degradation of DDT (1,1,1-trichloro-2,2-bis (4-chlorophenyl) ethane). The bacterium was able to degrade up to 42% of initial 50 mg L -1 of DDT within 10 days of incubation. The highlight of the work was the elucidation of DDT degradation pathway in S. marcescens. A total of four intermediates metabolites viz. 2,2-bis (chlorophenyl)-1,1-dichloroethane (DDD), 2,2-bis (chlorophenyl)-1,1-dichloroethylene (DDE), 2,2-bis (chlorophenyl)-1-chloroethylene (DDMU), and 4-chlorobenzoic acid (4-CBA) were identified by GC-Mass and FTIR. 4-CBA was found to be the stable product of DDT degradation. Metabolites preceding 4-CBA were not toxic to strain as reveled through luxuriant growth in presence of varying concentrations of exogenous DDD and DDE. However, 4-CBA was observed to inhibit the growth of bacterium. The DDT degrading efficiency of S. marcescens NCIM 2919 hence could be used in combination with 4-CBA utilizing strains either as binary culture or consortia for mineralization of DDT. Application of S. marcescens NCIM 2919 to DDT contaminated soil, showed 74.7% reduction of initial 12.0 mg kg -1 of DDT after 18-days of treatment.

  11. Crystal structures of 2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-ethoxyprop-2-en-1-ide and bis(2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-(dicyanomethylenepropane-1,3-diide

    Directory of Open Access Journals (Sweden)

    Zouaoui Setifi

    2015-05-01

    Full Text Available In 2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-ethoxyprop-2-en-1-ide, C10H9N2+·C9H5N4O−, (I, the ethyl group in the anion is disordered over two sets of atomic sites with occupancies 0.634 (9 and 0.366 (9, and the dihedral angle between the ring planes in the cation is 2.11 (7°. The two independent C(CN2 groups in the anion make dihedral angles of 10.60 (6 and 12.44 (4° with the central propenide unit, and the bond distances in the anion provide evidence for extensive electronic delocalization. In bis(2,2′-bipyridin-1-ium 1,1,3,3-tetracyano-2-(dicyanomethylenepropane-1,3-diide [alternative name bis(2,2′-bipyridin-1-ium tris(dicyanomethylenemethanediide], 2C10H9N2+·C10N62− (II, the dihedral angles between the ring planes in the two independent cations are 7.7 (2 and 10.92 (17°. The anion exhibits approximate C3 symmetry, consistent with extensive electronic delocalization, and the three independent C(CN2 groups make dihedral angles of 23.8 (2, 27.0 (3 and 27.4 (2° with the central plane. The ions in (I are linked by an N—H...N hydrogen bond and the resulting ion pairs are linked by two independent C—H...N hydrogen bonds, forming a ribbon containing alternating R44(18 and R44(26 rings, where both ring types are centrosymmetric. The ions in (II are linked by two independent N—H...N hydrogen bonds and the resulting ion triplets are linked by a C—H...N hydrogen bond, forming a C21(7 chain containing anions and only one type of cation, with the other cation linked to the chain by a further C—H...N hydrogen bond.

  12. Study of interactions between octyl-β-D-glucopyranoside and the hydroxyethyl-cellulose biopolymer in aqueous solution

    International Nuclear Information System (INIS)

    Villegas-Pañeda, Ximena; Pérez-Casas, Silvia; Hernández-Baltazar, Efrén; Chávez-Castellanos, Angel E.

    2014-01-01

    Graphical abstract: - Highlights: • Interactions in mixed micelles to be used as drug carriers were studied. • We tested this system to nanoencapsulate the metronidazole as a drug model. • Characteristic concentrations for the micelle formation process were obtained. • The micelles formation in all cases is spontaneous, and entropy driven. • Thermodynamic properties of demicellization for the mixed micelles were determined. - Abstract: (Surfactant + polymer) systems play an important role in drug delivery. They control the drug release rate by improving solubility, minimizing degradation, contributing to the reduction of toxicity and facilitating drug administration. Physicochemical properties of surfactant/polymer systems used in controlled drug release are affected by the composition of the mixture. The study of the physicochemical behavior of these mixtures allows the design of more suitable drug pharmaceutical formulation according to its chemical structure. In this paper, critical micelle concentration (CMC), saturation concentration (C 2 ), critical aggregation concentration (CAC) and thermodynamic parameters, such as enthalpy (ΔH), Gibbs free energy (ΔG) and the temperature multiplied by entropy (TΔS) for the demicellization process were determined by isothermal titration calorimetry (ITC), for octyl-β-D-glucopyranoside (OGP) and hydroxyethyl-cellulose (HEC) aqueous solutions in order to construct a phase diagram suitable for the study of the interactions in each region and to choose the appropriate system for drug delivery. The interpretation of the results is supported by the analysis of particle size measurements by dynamic light scattering (DLS)

  13. Synthesis of N-(5-(Substitutedphenyl-4,5-dihydro-1H-pyrazol-3-yl-4H-1,2,4-triazol-4-amine from 4-Amino-4H-1,2,4-triazole

    Directory of Open Access Journals (Sweden)

    Ashvin D. Panchal

    2011-01-01

    Full Text Available N-(4H-1,2,4-Triazol-4-ylacetamide (2 were prepared by reaction of 4-amino-4H-1,2,4-triazole (1 with acetyl chloride in dry benzene. It has been reacted with various aromatic aldehyde to afford 3-(substitutedphenyl-N-(4H-1,2,4-triazol-4-ylacrylamide (3a-e. The synthesis of N-(5-substitutedphenyl-4,5-dihydro-1H-pyrazol-3-yl-4H-1,2,4-triazol-4-amine (4a-e is achieved by the cyclisation of 3a-e with hydrazine hydrate in ethanol. The structures of synthesized compounds were characterized by 1H NMR and IR spectroscopic studies. The purity of the compounds was checked by thin layer chromatography.

  14. Thermogravimetric analysis, kinetic study, and pyrolysis-GC/MS analysis of 1,1'-azobis-1,2,3-triazole and 4,4'-azobis-1,2,4-triazole.

    Science.gov (United States)

    Jia, Chenhui; Li, Yuchuan; Zhang, Shujuan; Fei, Teng; Pang, Siping

    2018-03-01

    In general, the greater the number of directly linked nitrogen atoms in a molecule, the better its energetic performance, while the stability will be accordingly lower. But 1,1'-azobis-1,2,3-triazole (1) and 4,4'-azobis-1,2,4-triazole (2) show remarkable properties, such as high enthalpies of formation, high melting points, and relatively high stabilities. In order to rationalize this unexpected behavior of the two compounds, it is necessary to study their thermal decompositions and pyrolyses. Although a great deal of research has been focused on the synthesis and characterization of energetic materials with 1 and 2 as the backbone, a complete report on their fundamental thermodynamic parameters and thermal decomposition properties has not been published. Thermogravimetric-differential scanning calorimetry were used to obtain the thermal decomposition data of the title compounds. Kissinger and Ozawa-Doyle methods, the two selected non-isothermal methods, are presented for analysis of the solid-state kinetic data. Pyrolysis-gas chromatography/mass spectrometry was used to study the pyrolysis process of the title compounds. The DSC curves show that the thermal decompositions of 1 and 2 are at different heating rates involved a single exothermic process. The TG curves provide insight into the total weight losses from the compounds associated with this process. At different pyrolysis temperatures, the compositions and types of the pyrolysis products differ greatly and the pyrolysis reaction at 500 °C is more thorough than 400 °C. Apparent activation energies (E) and pre-exponential factors (lnA/s -1 ) are 291.4 kJ mol -1 and 75.53 for 1; 396.2 kJ mol -1 and 80.98 for 2 (Kissinger). The values of E are 284.5 kJ mol -1 for 1 and 386.1 kJ mol -1 for 2 (Ozawa-Doyle). The critical temperature of thermal explosion (T b ) is evaluated as 187.01 °C for 1 and 282.78 °C for 2. The title compounds were broken into small fragment ions under the pyrolysis conditions

  15. G 2.4 + 1.4: a supernova remnant or ring nebula around a peculiar star

    International Nuclear Information System (INIS)

    Johnson, H.M.

    1975-01-01

    G2.4+1.4 is a probable nonthermal radio source and an optical nebula which appears to be a supernova remnant (SNR). It also contains an O vi sequence star of great excitation. We present new radiofrequency continuum and (nil) H 92α observations, optical spectroscopy, and Fabry-Perot scanner observations of the nebula. The object distance (5 kpc), origin of gas kinematics (SNR expansion), and mode of excitation of the gas (photoexcitation and/or shock wave) remain uncertain. We discuss the possible roles of the O vi star as ''runaway'' in a SNR, as a source of photoexcitation, and as an ejector of a ''counterfeit'' SNR

  16. Synergistic complexes of uranyl ion with 1-phenyl-3-methyl-4-acetyl-pyrazolone-5 and some oxo-donors

    International Nuclear Information System (INIS)

    Nagar, M.S.; Ruikar, P.B.; Subramanian, M.S.

    1987-01-01

    Complexes of uranyl ion with 1-phenyl-3-methyl-4-acetyl-pyrazolone-5(PMAP) and various oxo-donors such as aliphatic sulphoxides [R 2 SO, where R = i-C 5 H 11 (DISO), n-C 6 H 13 (DHSO), n-C 7 H 15 (DSSO), n-C 8 H 17 (DOSO), n-C 9 H 19 (DNSO), n-C 10 H 21 (DDSO), n-C 11 H 23 (DUDSO) and n-C 4 H 9 (DBUSO)] tributylphosphate (TBP) and tri-n-octyl phosphine oxide (TOPO) have been synthesised and characterized. Analytical data establish that they have the stoichiometry UO 2 (PMAP) 2 X where X is the oxo-donor. The IR spectra of the sulphoxide complexes in the S - O stretching region indicate that the ligands R 2 SO are O-bonded. The methyl protons of the pyrazole ring and acetyl group in the PMAP ligand are equivalent giving rise to a single sharp peak in the PMR spectra, whereas in the synergistic complexes with the oxo-donors, two deshielded peaks of equal intensity are observed which indicate the non-equivalence of the methyl groups. The peak which is more deshielded has been ascribed to the methyl of the acetyl group. The higher deshielding of these methyl protons arises due to the transfer of electron density to the metal atom on complexation. (author)

  17. Fluorine Substituted 1,2,4-Triazinones as Potential Anti-HIV-1 and CDK2 Inhibitors

    Directory of Open Access Journals (Sweden)

    Mohammed S. I. Makki

    2014-01-01

    Full Text Available Fluorine substituted 1,2,4-triazinones have been synthesized via alkylation, amination, and/or oxidation of 6-(2-amino-5-fluorophenyl-3-thioxo-3,4-dihydro-1,2,4-triazin-5(2H-one 1 and 4-fluoro-N-(4-fluoro-2-(5-oxo-3-thioxo-2,3,4,5-tetrahydro-1,2,4-triazin-6-ylphenylbenzamide 5 as possible anti-HIV-1 and CDK2 inhibitors. Alkylation on positions 2 and 4 in 1,2,4-triazinone gave compounds 6–8. Further modification was performed by selective alkylation and amination on position 3 to form compounds 9–15. However oxidation of 5 yielded compounds 16–18. Structures of the target compounds have been established by spectral analysis data. Five compounds (5, 11, 14, 16, and 17 have shown very good anti-HIV activity in MT-4 cells. Similarly, five compounds (1, 3, and 14–16 have exhibited very significant CDK2 inhibition activity. Compounds 14 and 16 were found to have dual anti-HIV and anticancer activities.

  18. Density, dynamic viscosity, and electrical conductivity of pyridinium-based hydrophobic ionic liquids

    International Nuclear Information System (INIS)

    Liu, Qing-Shan; Li, Pei-Pei; Welz-Biermann, Urs; Chen, Jian; Liu, Xiao-Xia

    2013-01-01

    Highlights: • Targets of this research are hydrophobic series ionic liquids. • Density, dynamic viscosity and electrical conductivity were determined. • Influences of methylene to properties were discussed. • Influences of methyl group on pyridinium ring position to properties were discussed. • Relationship of ρ, η and σ were described systematically. -- Abstract: Air and water stable hydrophobic ionic liquids (ILs) were synthesized: N-propyl-3-methylpyridinium bis(trifluoromethylsulfonyl)imide [C 3 3mpy][NTf 2 ], N-hexyl-3-methylpyridinium bis(trifluoromethylsulfonyl)imide [C 6 3mpy][NTf 2 ], and N-hexyl-4-methylpyridinium bis(trifluoromethylsulfonyl)imide [C 6 4mpy][NTf 2 ]. Density, dynamic viscosity, and electrical conductivity of ILs were determined at atmospheric pressure in the temperature range of (278 to 353) K. The effects of methylene and methyl groups to density, dynamic viscosity, and electrical conductivity, respectively, were discussed. The thermal expansion coefficient, molecular volume, standard molar entropy, and lattice energy of the samples were estimated in terms of empirical and semi-empirical equations based on the density values. The temperature dependence on dynamic viscosity and electrical conductivity values of the ILs were discussed by Vogel–Fulcher–Tamman (VFT) and Arrhenius equations. The molar conductivities were calculated by density and electrical conductivity values

  19. Synthesis, physical-chemical properties of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acid esters

    Directory of Open Access Journals (Sweden)

    V. M. Odyntsova

    2017-04-01

    Full Text Available The nitrogen-containing heterocyclic systems from the class of 1,2,4-triazole derivatives, which exhibit wide range of actions, occupy special place among the variety of heterocyclic compounds. Derived biologically active substances are actively introduced into practice as new original and effective drugs. We were interested in esters of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids, which exhibit high biological activity and can be intermediates for the synthesis of amides, hydrazides, ylidenderivatives of corresponding acids. The aim of this work is the synthesis of new esters of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids and the establishment of their physical-chemical properties. Materials and methods. Melting point was determined by open capillary method on the device OptiMelt MPA100. The elemental composition of the synthesized compounds was determined on the universal analyzer ElementarVario ЕL cube (CHNS (standard – sulfanilamide. 1H NMR spectra were recorded on spectrometer Varian Mercury VX-200 (1H, 200 MHz in the solvent dimethyl sulfoxide-d6 (tetramethylsilane internal standard and decoded using a program ADVASP(tm Analyzer program (Umatek International Inc.. Chromato-mass-spectral studies were performed on hazarding chromatograph Agilent 1260 Infinity HPLC equipped with mass spectrometer Agilent 6120 (ionization electro-spray (ESI. The results and discussion. Synthesis of 11 new compounds, namely esters of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acids was carried out by two methods. According to the A method the alkylation of previously synthesized 3-(adamantan-1-yl-1H-1,2,4-triazole-5-thiol was performed with the use of corresponding methyl ester of 2-chloroacetic acid and the presence of equivalent amount of sodium hydroxide. The B method involves the etherification of 2-((5-(adamantan-1-yl-4-R-4H-1,2,4-triazole-3-ylthioacetic acid with the use of methyl, ethyl, i

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

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    Hind Jabli

    2010-01-01

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

  1. (2S,4R-2-[(1R-1-(4-Bromophenyl-2-nitroethyl]-4-ethylcyclohexanone

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    Chi-Xiao Zhang

    2013-02-01

    Full Text Available The crystal structure of the title compound, C16H20BrNO3, contains three chiral centers in the configuration 1R,2S,6R. The cyclohexane ring is in a chair conformation. In the crystal, molecules are linked by weak C—H...O interactions, forming chains along the a-axis direction.

  2. Enhanced CO2 capture in binary mixtures of 1-alkyl-3-methylimidazolium tricyanomethanide ionic liquids with water.

    Science.gov (United States)

    Romanos, George E; Zubeir, Lawien F; Likodimos, Vlassis; Falaras, Polycarpos; Kroon, Maaike C; Iliev, Boyan; Adamova, Gabriela; Schubert, Thomas J S

    2013-10-10

    Absorption of carbon dioxide and water in 1-butyl-3-methylimidazoliun tricyanomethanide ([C4C1im][TCM]) and 1-octyl-3-methylimidazolium tricyanomethanide ([C8C1im][TCM]) ionic liquids (ILs) was systematically investigated for the first time as a function of the H2O content by means of a gravimetric system together with in-situ Raman spectroscopy, excess molar volume (V(E)), and viscosity deviation measurements. Although CO2 absorption was marginally affected by water at low H2O molar fractions for both ILs, an increase of the H2O content resulted in a marked enhancement of both the CO2 solubility (ca. 4-fold) and diffusivity (ca. 10-fold) in the binary [C(n)C1im][TCM]/H2O systems, in contrast to the weak and/or detrimental influence of water in most physically and chemically CO2-absorbing ILs. In-situ Raman spectroscopy on the IL/CO2 systems verified that CO2 is physically absorbed in the dry ILs with no significant effect on their structural organization. A pronounced variation of distinct tricyanomethanide Raman modes was disclosed in the [C(n)C1im][TCM]/H2O mixtures, attesting to the gradual disruption of the anion-cation coupling by the hydrogen-bonded water molecules to the [TCM](-) anions, in accordance with the positive excess molar volumes and negative viscosity deviations for the binary systems. Most importantly, CO2 absorption in the ILs/H2O mixtures at high water concentrations revealed that the [TCM](-) Raman modes tend to restore their original state for the heavily hydrated ILs, in qualitative agreement with the intriguing nonmonotonous transients of CO2 absorption kinetics unveiled by the gravimetric measurements for the hybrid solvents. A molecular exchange mechanism between CO2 in the gas phase and H2O in the liquid phase was thereby proposed to explain the enhanced CO2 absorption in the hybrid [C(n)C1im][TCM]//H2O solvents based on the subtle competition between the TCM-H2O and TCM-CO2 interactions, which renders these ILs very promising for CO2

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

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    S. Gopinath

    2017-02-01

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

  4. Transmembrane and ubiquitin-like domain-containing protein 1 (Tmub1/HOPS facilitates surface expression of GluR2-containing AMPA receptors.

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    Hyunjeong Yang

    Full Text Available Some ubiquitin-like (UBL domain-containing proteins are known to play roles in receptor trafficking. Alpha-amino-3-hydroxy-5-methyl-4-isoxazole propionic acid receptors (AMPARs undergo constitutive cycling between the intracellular compartment and the cell surface in the central nervous system. However, the function of UBL domain-containing proteins in the recycling of the AMPARs to the synaptic surface has not yet been reported.Here, we report that the Transmembrane and ubiquitin-like domain-containing 1 (Tmub1 protein, formerly known as the Hepatocyte Odd Protein Shuttling (HOPS protein, which is abundantly expressed in the brain and which exists in a synaptosomal membrane fraction, facilitates the recycling of the AMPAR subunit GluR2 to the cell surface. Neurons transfected with Tmub1/HOPS-RNAi plasmids showed a significant reduction in the AMPAR current as compared to their control neurons. Consistently, the synaptic surface expression of GluR2, but not of GluR1, was significantly decreased in the neurons transfected with the Tmub1/HOPS-RNAi and increased in the neurons overexpressing EGFP-Tmub1/HOPS. The altered surface expression of GluR2 was speculated to be due to the altered surface-recycling of the internalized GluR2 in our recycling assay. Eventually, we found that GluR2 and glutamate receptor interacting protein (GRIP were coimmunoprecipitated by the anti-Tmub1/HOPS antibody from the mouse brain. Taken together, these observations show that the Tmub1/HOPS plays a role in regulating basal synaptic transmission; it contributes to maintain the synaptic surface number of the GluR2-containing AMPARs by facilitating the recycling of GluR2 to the plasma membrane.

  5. 1,1′,4,5-Tetrahydrotrispiro[1,3,2-diazaphosphole-2,2′-[1,3,5,2,4,6]triazatriphosphinine-4′,6′′-dibenzo[d,f][1,3,2]dioxaphosphepine-6′,6′′′-dibenzo[d,f][1,3,2]dioxaphosphepine] acetone monosolvate

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    Krystal R. Fontenot

    2013-09-01

    Full Text Available The title compound, C26H22N5O4P3·C3H6O, has been achieved in a two-step synthesis that does not require chromatography. This molecule contains a seven-membered spirocyclic ring at two P-atom positions and a five-membered ring containing new P—N bonds at the other P-atom position. Endocyclic torsion angles about the central biphenyl C—C bonds are −41.5 (3 and −44.4 (3°, and P—N bonds of the central P3N3 ring are within the range 1.5665 (17–1.6171 (17 Å, while the P—O distances are in the range 1.5940 (14–1.6041 (14 Å. One N—H group makes an intermolecular N—H...N hydrogen bond, forming centrosymmetric dimers, while the other N—H group makes an N—H...O hydrogen bond to the acetone solvent molecule. The crystal was a two-component non-merohedral twin with ratio 0.811/0.189.

  6. Simple and Efficient Synthesis of Racemic 2-(tert-Butoxycarbon-ylamino-2-methyl-3-(1H-1,2,4-triazol-1-ylpropanoic Acid, a New Derivative of β-(1,2,4-Triazol-1-ylalanine

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    Abdelali Kerbal

    2011-04-01

    Full Text Available A simple synthetic approach to racemic N-tert-butyloxycarbonyl-2-methyl-3-(1H-1,2,4-triazol-1-ylalanine (5 in four steps and 68% overall yield starting from oxazoline derivative 1 is reported. This synthesis involves the alkylation of 1H-1,2,4-triazole with an O-tosyloxazoline derivative, followed by an oxazoline ring-opening reaction and oxidation of the N-protected β‑aminoalcohol by potassium permanganate.

  7. Crystal structure of 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl) ethenyl]benzamide: N,N-dimethylformamide (1 : 1)

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, P. [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India); Subbulakshmi, K. N.; Narayana, B. [Mangalore University, Department of Chemistry (India); Sarojini, B. K. [Mangalore University, Industrial Chemistry Division, Department of Studies in Chemistry (India); Kant, R., E-mail: rkant.ju@gmail.com [University of Jammu, X-ray Crystallography Laboratory, Department of Physics (India)

    2016-03-15

    The title compound, 2-(thiophen-2-yl)-1-(5-thioxo-4,5-dihydro-1,3,4-oxadiazol-2-yl)ethenyl] benzamide:N,N-dimethylformamide (1: 1), (C{sub 15}H{sub 11}N{sub 3}O{sub 2}S{sub 2} · C{sub 3}H{sub 7}NO), was synthesized, and its structure was established by spectral analysis and X-ray diffraction studies. The compound crystallizes in the monoclinic space group P2{sub 1}/n with a = 10.8714(7), b = 9.0497(5), c = 19.8347(13) Å, β = 91.093(5)°, Z = 4. The crystal structure is stabilized by N–H···S, C–H···O and N–H···O hydrogen bonds. The π···π interactions are also observed between the rings.

  8. New coordination polymers from 1D chain, 2D layer to 3D framework constructed from 1,2-phenylenediacetic acid and 1,3-bis(4-pyridyl)propane flexible ligands

    Science.gov (United States)

    Xin, Ling-Yun; Liu, Guang-Zhen; Wang, Li-Ya

    2011-06-01

    The hydrothermal reactions of Cd, Zn, or Cu(II) acetate salts with H 2PHDA and BPP flexible ligands afford three new coordination polymers, including [Cd(PHDA)(BPP)(H 2O)] n(1), [Zn(PHDA)(BPP)] n(2), and [Cu 2(PHDA) 2(BPP)] n(3) (H 2PHDA=1,2-phenylenediacetic acid, BPP=1,3-bis(4-pyridyl)propane). The single-crystal X-ray diffractions reveal that all three complexes feature various metal carboxylate subunits extended further by the BPP ligands to form a diverse range of structures, displaying a remarked structural sensitivity to metal(II) cation. Complex 1 containing PHDA-bridged binuclear cadmium generates 1D double-stranded chain, complex 2 results in 2D→2D interpenetrated (4,4) grids, and complex 3 displays a 3D self-penetrated framework with 4 86 68 rob topology. In addition, fluorescent analyses show that both 1 and 2 exhibit intense blue-violet photoluminescence in the solid state.

  9. Polymer Inclusion Membrane Containing a Tripodal Diglycolamide Ligand: Actinide Ion Uptake and Transport Studies

    NARCIS (Netherlands)

    Mahanty, B.; Mohapatra, P.K.; Raut, D.R.; Das, D.K.; Behere, P.G.; Afzal, M.; Verboom, Willem

    2016-01-01

    A cellulose triacetate (CTA)-based polymer inclusion membrane (PIM) containing a C-pivot tripodal diglycolamide (T-DGA) as the carrier extractant and 2-nitrophenyl octyl ether (NPOE) as the plasticizer shows potential for the uptake of actinides from acidic feed solutions. The uptake of actinides

  10. Poly[4,4'-(propane-1,3-diyl)dipyridinium bis{tetraaquabis(μ2-5-carboxybenzene-1,2,4-tricarboxylato)bis[μ2-1,3-bis(4-pyridyl)propane]dicobalt(II)} pentahydrate].

    Science.gov (United States)

    Atria, Ana María; Corsini, Gino; Garland, Maria Teresa; Baggio, Ricardo

    2011-11-01

    The title polymeric compound, {(C(13)H(16)N(2))[Co(C(10)H(3)O(8))(C(13)H(14)N(2))(H(2)O)(2)](2)·5H(2)O}(n), is an ionic structure comprising an anionic two-dimensional mesh characterized by a {[Co(Hbtc)(bpp)(H(2)O)(2)](-)}(2) motif [Hbtc is 5-carboxybenzene-1,2,4-tricarboxylate and bpp is 1,3-bis(4-pyridyl)propane], with interspersed 4,4'-(propane-1,3-diyl)dipyridinium cations, denoted (H(2)bpp)(2+), and water molecules providing the charge balance and structure stabilization. The reticular mesh consists of two independent types of [Co(H(2)O)(2)](2+) cationic nodes (lying on inversion centres), interconnected in the [101] direction by two independent sets of neutral bridging bpp ligands, both types of ligands being split by non-equivalent twofold axes. One set is formed by genuinely symmetric moieties, while those in the second set are only symmetric by disorder in the central propane bridge. These chains contain only one type of Co(II) centre and one type of bpp ligand; the metal cations therein are laterally bridged by Hbtc anions, thus forming transverse chains of alternating types of Co(II) cations. The elemental motif of the resulting grid is a highly distorted parallelogram, with metal-metal distances of 13.5242 (14) Å in the bpp direction and 9.105 (2) Å in the Hbtc direction, and a large internal angle of 138.42 (18)°. These two-dimensional structures have a profusion of hydrogen-bonding interactions with each other, either directly (with the aqua molecules as donors and the Hbtc anions as acceptors) or mediated by the unbound (H(2)bpp)(2+) cations and water molecules of hydration. These interactions generate a very complex hydrogen-bonding scheme involving all of the available N-H and O-H groups and which links these two-dimensional grids into a three-dimensional network.

  11. Overexpression of octamer transcription factors 1 or 2 alone has no effect on HIV-1 transcription in primary human CD4 T cells

    International Nuclear Information System (INIS)

    Zhang Mingce; Genin, Anna; Cron, Randy Q.

    2004-01-01

    We explored the binding of octamer (Oct) transcription factors to the HIV-1 long terminal repeat (LTR) by gel shift assays and showed none of the previously identified four potential Oct binding sites bound Oct-1 or Oct-2. Overexpression of Oct-1 or Oct-2 had no effect on HIV-1 LTR activity in transiently transfected primary human CD4 T cells. Next, primary human CD4 T cells were co-transfected with a green fluorescent protein (GFP)-expression vector and an Oct-1 or Oct-2 expression plasmid. The transfected cells were stimulated for 2 days and then infected with the NL4-3 strain of HIV-1. After 3 days of infection, there were no differences in HIV-1 p24 supernatant levels. Apoptosis of infected or bystander cells overexpressing Oct-1 or Oct-2 compared to control was also unaffected. Our studies demonstrate that Oct-1 and Oct-2 fail to bind to the HIV-1 LTR and have no effect on HIV-1 transcription in primary human CD4 T cells

  12. Poly[dibromidobis[μ-1-(pyridin-4-ylmethyl-1H-1,2,4-triazole-κ2N:N′]cadmium

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    Xiu-Zhi Xu

    2011-02-01

    Full Text Available The title coordination polymer, [CdBr2(C8H8N42]n, arose from a layer-separated diffusion synthesis at room temperature. The title compound is isotypic with the I and Cl analogues. The Cd atom, located on an inversion center, is coordinated by two bromide ions and four N atoms (two from triazole rings and two from pyridyl rings in a distorted trans-CdBr2N4 octahedral arrangement. The bridging 1-(4-pyridylmethyl-1H-1,2,4-triazole ligands are twisted [dihedral angle between the triazole and pyridine rings = 72.56 (13°], affording a two-dimensional 44 sheet structure in the crystal.

  13. 2-Aminobenzoic acid–4-(pyridin-4-yldisulfanylpyridine (1/1

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    Hadi D. Arman

    2011-12-01

    Full Text Available The title 1:1 co-crystal, C7H7NO2·C10H8N2S2, features a highly twisted 4-(pyridin-4-yldisulfanylpyridine molecule [dihedral angle between the pyridine rings = 89.06 (10°]. A small twist is evident in the 2-aminobenzoic acid molecule, with the C—C—C—O torsion angle being −7.7 (3°. An N—H...O hydrogen bond occurs in the 2-aminobenzoic acid molecule. In the crystal, molecules are linked by O—H...N and N—H...N hydrogen bonds into a supramolecular chain along the b axis. These are connected into layers by π–π interactions occurring between pyridine rings [centroid–centroid distance = 3.8489 (15 Å]. The layers are connected along the a axis by C—H...O contacts. The crystal studied was a racemic twin.

  14. Crystal structures of 1,4-diazabicyclo[2.2.2]octan-1-ium 4-nitrobenzoate dihydrate and 1,4-diazabicyclo[2.2.2]octane-1,4-diium bis(4-nitrobenzoate: the influence of solvent upon the stoichiometry of the formed salt

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    Aina Mardia Akhmad Aznan

    2014-07-01

    Full Text Available The 1:1 co-crystallization of 1,4-diazabicyclo[2.2.2]octane (DABCO with 4-nitrobenzoic acid in ethanol–water (3/1 gave the salt dihydrate C6H13N2+·C7H4NO4−·2H2O, (1, whereas from methanol, the salt C6H14N22+·2C7H4NO4−, (2, was isolated. In (1, the cation and anion are linked by a strong N—H...O hydrogen bond, and the carboxylate anion is close to planar [dihedral angle between terminal residues = 6.83 (9°]. In (2, a three-ion aggregate is assembled by two N—H...O hydrogen bonds, and the carboxylate anions are again close to planar [dihedral angles between terminal residues = 1.7 (3 and 5.9 (3°]. Through the intervention of solvent water molecules, which self-assemble into helical supramolecular chains along the b axis, the three-dimensional architecture in (1 is stabilized by water–DABCO O—H...N and water–carboxylate O—H...O hydrogen bonds, with additional stability afforded by C—H...O interactions. The global crystal structure comprises alternating layers of water molecules and ion pairs stacked along the c axis. In the crystal of (2, the three-ion aggregates are assembled into a three-dimensional architecture by a large number of methylene–carboxylate/nitro C—H...O interactions as well as π–π contacts between inversion-related benzene rings [inter-centroid distances = 3.5644 (16 and 3.6527 (16 Å]. The cations and anions assemble into alternating layers along the c axis.

  15. Anticonvulsant activity of a mGlu(4alpha) receptor selective agonist, (1S,3R,4S)-1-aminocyclopentane-1,2,4-tricarboxylic acid.

    Science.gov (United States)

    Chapman, A G; Talebi, A; Yip, P K; Meldrum, B S

    2001-07-20

    The metabotropic Group III agonist, (1S,3R,4S)-1-aminocyclopentane-1,2,4-tricarboxylic acid (ACPT-1), selective for the mGlu(4alpha) receptor, suppresses sound-induced seizures in DBA/2 mice following its intracerebroventricular (i.c.v.) administration (ED(50) 5.6 [2.9-10.7], nmol i.c.v., 15 min, clonic phase) and in genetically epilepsy-prone (GEP) rats following focal administration into the inferior colliculus (ED(50) 0.08 [0.01-0.50], nmol, 60 min, clonic phase). ACPT-1 also protects against clonic seizures induced in DBA/2 mice by the Group I agonist, (RS)-3,5-dihydroxyphenylglycine (3,5-DHPG) (ED(50) 0.60 [0.29-1.2], nmol i.c.v.) and by the Group III antagonist, (RS)-alpha-methylserine-O-phosphate (MSOP) (ED(50) 49.3 [37.9-64.1], nmol i.c.v.). Another Group III agonist, (RS)-4-phosphonophenyl-glycine (PPG), preferentially activating the mGlu(8) receptor, previously shown to protect against sound-induced seizures in DBA/2 mice and GEP rats, also protects against seizures induced in DBA/2 by 3,5-DHPG (ED(50) 3.7 [2.4-5.7], nmol i.c.v.) and by the Group III antagonist, MSOP (ED(50) 40.2 [21.0-77.0], nmol i.c.v.). At very high doses (500 nmol i.c.v. and above), Group III antagonists have pro-convulsant and convulsant activity. The anticonvulsant protection against sound-induced seizures in DBA/2 mice provided by a fully protective dose (20 nmol, i.c.v.) of the mGlu(4) receptor agonist ACPT-1, is partially reversed by the co-administration of the Group III antagonists, MSOP, (RS)-alpha-methyl-4-phosphonophenylglycine (MPPG) or (S)-2-amino-2-methyl-4-phosphonobutanoic acid (MAP4), in the 20-50 nmol dose range. At doses of 50-200 nmol, MPPG and MAP4 cause further reversal of the ACPT-1 anticonvulsant protection, while the MSOP effect on ACPT-1 protection is abolished at higher doses. In contrast, the anticonvulsant protection against sound-induced seizures in DBA/2 mice provided by a fully protective dose (20 nmol, i.c.v.) of the mGlu(8) receptor agonist PPG, is not

  16. (2E-3-(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-yl-1-(2,5-dimethyl-3-thienylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    Salman A. Khan

    2010-04-01

    Full Text Available The title compound, (2E-3-(3,5-dimethyl-1-phenyl-1H-pyrazol-4-yl-1-(2,5-dimethyl-3-thienylprop-2-en-1-one (3 was synthesized in high yield by aldol condensation of 3-acetyl-2,5-dimethylthiophene and 3,5-dimethyl-1-phenylpyrazole-4-carboxaldehyde in ethanolic NaOH at room temperature. Its structure was fully characterized by elemental analysis, IR, 1H NMR, 13C NMR and EI-MS spectral analysis.

  17. Use of 2-octyl cyanoacrylate adhesive in rat liver induced lesion Uso adesivo de 2-octil cianoacrilato em lesão induzida de fígado de ratos

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    Orlando José dos Santos

    2012-09-01

    Full Text Available PURPOSE: To evaluate the healing process of rat traumatic liver lesion corrected with the use of 2-octyl cyanoacrylate adhesive, compared to the use of biologically absorbable chromed catgut thread suture. METHODS: Thirty mail adult rats were divided into two groups (15 per group according to the used method for liver lesion correction as follows: adhesive group (AG, and catgut group (CG; each group being divided into three subsets of five animals (7th, 14th, and 21st day, respectively, according to post-surgery evaluation. All animals were submitted to homogeneous lesion applying synthetic bonding to AG and using chromed catgut suture to CG for lesion correction. Macroscopic and microscopic parameters of healing processes were evaluated. RESULTS: Both groups of animals showed excellent abdominal wall healing, with no evidence of infection, and no abdominal cavity peritonitis or abscess. The presence of adherence was observed in both groups with no statistically significant difference. As to macroscopic evaluation, there was statistically significant difference with respect to specific factors of clinical inflammation (ischemic inflammation and giant celular inflammatory reaction between animals evaluated on the 10th day (ischemic necrosis and giant celular inflammatory reaction among animals evaluated on the 14th day (A14 versus C14. CONCLUSION: Applying 2-octyl-cyanoacrylate adhesive for correcting rat liver lesion does not change healing process when compared to the use of chromed catgut stitch.OBJETIVO: Avaliar o processo de cicatrização de lesão induzida em fígado de rato utilizando adesivo de 2-octil cianoacrilato em comparação com a sutura com catgut cromado. MÉTODOS: Utilizou-se 30 ratos adultos, machos, distribuídos em dois grupos de 15 animais denominados de grupo adesivo (GA e grupo catgut (GC; cada grupo foi dividido em três subgrupos, cada um com cinco animais, de acordo com a data marcada para avaliação p

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

    Directory of Open Access Journals (Sweden)

    Hamad Mohamed Al-Matar

    2010-05-01

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

  19. (E-2-((4R,5R-5-((Benzyloxymethyl-2,2-dimethyl-1,3-dioxolan-4-ylbut-2-ene-1,4-diol

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    Carlos R. Carreras

    2010-04-01

    Full Text Available The synthesis of (E-2-((4R,5R-5-((benzyloxymethyl-2,2-dimethyl-1,3-dioxolan-4-ylbut-2-ene-1,4-diol by a one-step reduction of the appropriate 2-substituted butenolide is reported. Product characterization was carried out by IR, 1H NMR, 13C NMR, MS, elemental analysis and optical rotation.

  20. Weapon container catalog. Volumes 1 & 2

    Energy Technology Data Exchange (ETDEWEB)

    Brown, L.A.; Higuera, M.C.

    1998-02-01

    The Weapon Container Catalog describes H-gear (shipping and storage containers, bomb hand trucks and the ancillary equipment required for loading) used for weapon programs and for special use containers. When completed, the catalog will contain five volumes. Volume 1 for enduring stockpile programs (B53, B61, B83, W62, W76, W78, W80, W84, W87, and W88) and Volume 2, Special Use Containers, are being released. The catalog is intended as a source of information for weapon program engineers and also provides historical information. The catalog also will be published on the SNL Internal Web and will undergo periodic updates.

  1. Toxicological evaluation of two novel bitter modifying flavour compounds: 3-(1-((3,5-dimethylisoxazol-4-ylmethyl-1H-pyrazol-4-yl-1-(3-hydroxybenzylimidazolidine-2,4-dione and 3-(1-((3,5-dimethylisoxazol-4-ylmethyl-1H-pyrazol-4-yl-1-(3-hydroxybenzyl-5,5-dimethylimidazolidine-2,4-dione

    Directory of Open Access Journals (Sweden)

    Donald S. Karanewsky

    Full Text Available A toxicological evaluation of two novel bitter modifying flavour compounds, 3-(1-((3,5-dimethylisoxazol-4-ylmethyl-1H-pyrazol-4-yl-1-(3-hydroxybenzylimidazolidine-2,4-dione (S6821, CAS 1119831-25-2 and 3-(1-((3,5-dimethylisoxazol-4-ylmethyl-1H-pyrazol-4-yl-1-(3-hydroxybenzyl-5,5-dimethylimidazolidine-2,4-dione (S7958, CAS 1217341-48-4, were completed for the purpose of assessing their safety for use in food and beverage applications. S6821 undergoes oxidative metabolism in vitro, and in rat pharmacokinetic studies both S6821 and S7958 are rapidly converted to the corresponding O-sulfate and O-glucuronide conjugates. S6821 was not found to be mutagenic or clastogenic in vitro, and did not induce micronuclei in bone marrow polychromatic erythrocytes in vivo. S7958, a close structural analog of S6821, was also found to be non-mutagenic in vitro. In short term and subchronic oral toxicity studies in rats, the no-observed-adverse-effect-level (NOAEL for both S7958 and S6821 was 100 mg/kg bw/day (highest dose tested when administered as a food ad-mix for either 28 or 90 consecutive days, respectively. Furthermore, S6821 demonstrated a lack of maternal toxicity, as well as adverse effects on fetal morphology at the highest dose tested, providing a NOAEL of 1000 mg/kg bw/day for both maternal toxicity and embryo/fetal development when administered orally during gestation to pregnant rats. Keywords: S6821, S7958, FEMA GRAS, Subchronic toxicological evaluation, Genetic toxicological evaluation

  2. Synthesis and Biological Activity of Substituted Urea and Thiourea Derivatives Containing 1,2,4-Triazole Moieties

    Directory of Open Access Journals (Sweden)

    David E. Wedge

    2013-03-01

    Full Text Available A series of novel thiourea and urea derivatives containing 1,2,4-triazole moieties were synthesized and evaluated for their antifungal and larvicidal activity. Triazole derivatives 3a–e and 4a–e were synthesized by reacting thiocarbohydrazide with thiourea and urea compounds 1a–e and 2a–e, respectively, in a 130–140 °C oil bath. The proposed structures of all the synthesized compounds were confirmed using elemental analysis, UV, IR, 1H-NMR and mass spectroscopy. All compounds were evaluated for antifungal activity against plant pathogens, larvicidal and biting deterrent activity against the mosquito Aedes aegypti L. and in vitro cytotoxicity and anti-inflammatory activity against some human cell lines. Phomopis species were the most sensitive fungi to these compounds. Compounds 1b, 1c, 3a and 4e demonstrated selectively good activity against Phomopis obscurans and only 1b and 4e showed a similar level of activity against P. viticola. Compound 3d, with a LD50 value of 67.9 ppm, followed by 1c (LD50 = 118.8 ppm and 3e (LD50 = 165.6 ppm, showed the highest toxicity against Aedes aegypti larvae. Four of these compounds showed biting deterrent activity greater than solvent control, with the highest activity being seen for 1c, with a proportion not biting (PNB value of 0.75, followed by 1e, 2b and 1a. No cytotoxicity was observed against the tested human cancer cell lines. No anti-inflammatory activity was observed against NF-kB dependent transcription induced by phorbol myristate acetate (PMA in human chondrosarcoma cells.

  3. Benzene-1,2-dicarboxylic acid–pyridinium-2-olate (1/1

    Directory of Open Access Journals (Sweden)

    Chua-Hua Yu

    2012-07-01

    Full Text Available The asymmetric unit of the title compound, C5H5NO·C8H6O4, contains one o-phthalate acid molecule and one pyridin-2-ol molecule, which exists in a zwitterionic form. In the o-phthalate acid molecule, the carboxylate groups are twisted from the benzene ring by dihedral angles of 13.6 (1° and 73.1 (1°; the hydroxy H atom in the latter group is disordered over two positons in a 1:1 ratio. In the crystal, O—H...O and N—H...O hydrogen bonds link the molecules into zigzag chains in [-101].

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

    Directory of Open Access Journals (Sweden)

    Ghulam Fareed

    2012-05-01

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

  5. 1,4,2-Benzo/pyridodithiazine 1,1-dioxides structurally related to the ATP-sensitive potassium channel openers 1,2,4-Benzo/pyridothiadiazine 1,1-dioxides exert a myorelaxant activity linked to a distinct mechanism of action.

    Science.gov (United States)

    Pirotte, Bernard; de Tullio, Pascal; Florence, Xavier; Goffin, Eric; Somers, Fabian; Boverie, Stéphane; Lebrun, Philippe

    2013-04-25

    The synthesis of diversely substituted 3-alkyl/aralkyl/arylamino-1,4,2-benzodithiazine 1,1-dioxides and 3-alkylaminopyrido[4,3-e]-1,4,2-dithiazine 1,1-dioxides is described. Their biological activities on pancreatic β-cells and on smooth muscle cells were compared to those of the reference ATP-sensitive potassium channel (KATP channel) openers diazoxide and 7-chloro-3-isopropylamino-4H-1,2,4-benzothiadiazine 1,1-dioxide. The aim was to assess the impact on biological activities of the replacement of the 1,2,4-thiadiazine ring by an isosteric 1,4,2-dithiazine ring. Most of the dithiazine analogues were found to be inactive on the pancreatic tissue, although some compounds bearing a 1-phenylethylamino side chain at the 3-position exerted a marked myorelaxant activity. Such an effect did not appear to be related to the opening of KATP channels but rather reflected a mechanism of action similar to that of calcium channel blockers. Tightly related 3-(1-phenylethyl)sulfanyl-4H-1,2,4-benzothiadiazine 1,1-dioxides were also found to exert a pronounced myorelaxant activity, resulting from both a KATP channel activation and a calcium channel blocker mechanism. The present work highlights the critical importance of an intracyclic NH group at the 4-position, as well as an exocyclic NH group linked to the 3-position of the benzo- and pyridothiadiazine dioxides, for activity on KATP channels.

  6. Densities and speeds of sound for binary mixtures of (1,3-dioxolane or 1,4-dioxane) with (2-methyl-1-propanol or 2-methyl-2-propanol) at the temperatures (298.15 and 313.15) K

    International Nuclear Information System (INIS)

    Villares, A.; Martin, S.; Haro, M.; Giner, B.; Artigas, H.

    2004-01-01

    This paper reports densities and speeds of sound for the binary mixtures of (1,3-dioxolane or 1,4-dioxane) with (2-methyl-1-propanol or 2-methyl-2-propanol) at the temperatures (298.15 and 313.15) K. Excess volumes and excess isentropic compressibility coefficients have been calculated from experimental data and fitted by means of a Redlich-Kister type equation. The ERAS model has been used to calculate the excess volumes of the four systems at both temperatures

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

    Directory of Open Access Journals (Sweden)

    Bao-Yong Zhu

    2010-10-01

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

  8. Synthesis of thin film containing 4-amino-1,2,4-triazole iron(II) complexes

    Energy Technology Data Exchange (ETDEWEB)

    Onggo, Djulia, E-mail: djulia@Chem.itb.ac.id [Inorganic and Physical Chemistry Research Group, Faculty of Mathematics and Natural Sciences, Institut Teknologi Bandung, Jl. Ganesha 10 Bandung 40132 (Indonesia)

    2014-03-24

    The Iron(II) complex with 4-amino-1,2,4 triazole (NH{sub 2}-trz) ligand has potential applications as smart material since the compounds show a distinct color change from lilac at low temperature to colorless at high temperature. The lilac color of the complex represent the diamagnetic low spin state while the colorless correspond to the paramagnetic high spin state of iron(II). The transition between the two states could be tuned by changing the anionic group. Generally, the complex was synthesized directly from aqueous solution of iron(II) salt with considerable amounts of NH{sub 2}-trz solution produced solid powder compound. For application as an electronic molecular device, the complex should be obtained as a thin film. The transparent [Fe(NH{sub 2}trz){sub 3}]-Nafion film has been successfully obtained, however, no anion variation can be produced since the nafion is an anionic resin. In this work, the [Fe(NH{sub 2}trz){sub 3}]-complexes with several anions have been synthesized inside nata de coco membrane that commonly used as a medium for deposition metal nano-particles. After drying the membrane containing the complex became a thin film. At room temperature, the film containing iron(II) complexes of sulphate and nitrate salts show lilac color, similar to that of the original complexes in the powder form. On heating, the color of the complex film changed to colorless and this color change was observed reversibly. In contrast, the films containing perchlorate and tetrafluoroborate iron(II) complexes are colorless at room temperature and changed to lilac on cooling. The significant color changing of the iron(II)complexes in the nata de coco film can be used for demonstration thermo chromic effect of smart materials with relatively small amount of the compounds.

  9. 2-Aminobenzoic acid–4-(pyridin-4-yldisulfanyl)pyridine (1/1)

    OpenAIRE

    Hadi D. Arman; Trupta Kaulgud; Edward R. T. Tiekink

    2011-01-01

    The title 1:1 co-crystal, C7H7NO2·C10H8N2S2, features a highly twisted 4-(pyridin-4-yldisulfanyl)pyridine molecule [dihedral angle between the pyridine rings = 89.06 (10)°]. A small twist is evident in the 2-aminobenzoic acid molecule, with the C—C—C—O torsion angle being −7.7 (3)°. An N—H...O hydrogen bond occurs in the 2-aminobenzoic acid molecule. In the crystal, molecules are linked by O&#...

  10. IONIC LIQUID-CATALYZED ALKYLATION OF ISOBUTANE WITH 2-BUTENE

    Science.gov (United States)

    A detailed study of the alkylation of isobutane with 2-butene in ionic liquid media has been conducted using 1-alkyl-3-methylimidazolium halides?aluminum chloride encompassing various alkyl groups (butyl-, hexyl-, and octyl-) and halides (Cl, Br, and I) on its cations and anions,...

  11. Heteroaromatization with 4-Hydroxycoumarin Part II: Synthesis of Some New Pyrano[2,3-d]pyrimidines, [1,2,4]triazolo[1,5-c]pyrimidines and Pyrimido[1,6-b]-[1,2,4]triazine Derivatives

    Directory of Open Access Journals (Sweden)

    A. H. Bedair

    2001-05-01

    Full Text Available A variety of novel [1,2,4]triazolo[1,5-c]pyrimidine-13-ones (4a-f and (5b-d could be obtained via reaction of 9-amino-7-(4’-chlorophenyl-8,9-dihydro-8-imino-6H,7H-[1]benzopyrano[3`,4`:5,6]pyrano[2,3-d]pyrimidine-6-one (3 with a variety of reagents. Pyrano[2,3-d]pyrimidine-6-ones 5a, 8a-c and pyrimido[1,6-b][1,2,4]-triazine-3,14-dione (6 were also prepared. The antimicrobial activity of some of the synthesized compounds was tested.

  12. Comparative in vitro effects of 2,3,7,8-tetrachlorodibenzo-p-dioxin and selected polynuclear aromatic hydrocarbons on cyp1a1 gene transcription in cells which contain or are deficient in the 4S binding protein

    International Nuclear Information System (INIS)

    Kamps, C.; Safe, S.

    1990-01-01

    Using [ 3 H]-benzo[a]pyrene as the radioligand, several cell culture lines have been screened for the presence (or absence) of the 4S binding protein. Murine Hepa 1c1c7 cells contained both the 4S binding protein and the 9S (Ah) receptor whereas only the 9S receptor was detected in rat hepatoma H-4-II E cells in culture. The effects of a series of polynuclear aromatic hydrocarbons (PAHs) which included benzo[e]pyrene, benzo[ghi]perylene and 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and their interactive effects on CYP1A1 gene transcription was determined by Northern analysis in both cell lines. The results showed that the PAHs which exhibited high affinity for the 4S binding protein were inactive as inducers in both cell lines; TCDD was active in both cell lines and the interactive effects between the PAHs and TCDD did not significantly modulate TCDD-mediated CYP1A1 gene transcription. The results suggest that the 4S binding protein does not regulate CYP1A1 gene transcription

  13. Privileged scaffolds or promiscuous binders: a glance of pyrrolo[2,1-f][1,2,4]triazines and related bridgehead nitrogen heterocycles in medicinal chemistry.

    Science.gov (United States)

    Song, Yu'ning; Zhan, Peng; Zhang, Qingzhu; Liu, Xinyong

    2013-01-01

    Pyrrolo[2,1-f][1,2,4]triazine template, a unique bridgehead nitrogen heterocycle, certainly deserves the title of "privileged scaffold" in the drug discovery field because of the versatility and potential to yield derivatives with a wide range of biological activities, such as anti-anaplastic lymphoma kinase (ALK), Janus kinase 2 (JAK2), VEGFR-2, EGFR and/or HER2, Met kinase, p38α mitogen-activated protein (MAP) kinase and insulin-like growth factor receptor (IGF-1R) kinase activities, etc. These different biological properties of pyrrolo[2,1-f][1,2,4]triazine derivatives have motivated new studies in searching for novel derivatives with improved activity and also other applications in pharmaceutical field. However, no systematic review is available in the literature on the pyrrolo[2,1- f][1,2,4]triazine derivatives concerning the design of potent drug-like compounds. Owing to the importance of this heterocyclic system, the present paper is an attempt to the pharmacological activities, structural modifications and the structure-activity relationship (SAR) reported for bridgehead nitrogen heterocycles in the current literature, making an effort to highlight the importance and therapeutic potentials of the pyrrolo[2,1-f][1,2,4]triazine scaffold and its bridgehead nitrogen bioisosters as heterocyclic privileged medicinal scaffolds.

  14. 5-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione

    Directory of Open Access Journals (Sweden)

    Salman A. Khan

    2010-03-01

    Full Text Available The title compound, 5-[(3,5-dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]-1,3-diethyl-2-thioxodihydropyrimidine-4,6(1H,5H-dione, has been synthesized by condensation of 1,3-diethyl-2-thiobarbituric acid and 3,5-dimethyl-1-phenylpyrazole-4-carbaldehyde in ethanol in the presence of pyridine. The structure of this new compound was confirmed by elemental analysis, IR, 1H-NMR, 13C-NMR and EI-MS spectral analysis.

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

    Science.gov (United States)

    Baillargeon, Renee

    1987-01-01

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

  16. Cloning, purification and crystallization of Thermus thermophilus proline dehydrogenase

    International Nuclear Information System (INIS)

    White, Tommi A.; Tanner, John J.

    2005-01-01

    Cloning, purification and crystallization of T. thermophilus proline dehydrogenase is reported. The detergent n-octyl β-d-glucopyranoside was used to reduce polydispersity, which enabled crystallization. Nature recycles l-proline by converting it to l-glutamate. This four-electron oxidation process is catalyzed by the two enzymes: proline dehydrogenase (PRODH) and Δ 1 -pyrroline-5-carboxylate dehydrogenase. This note reports the cloning, purification and crystallization of Thermus thermophilus PRODH, which is the prototype of a newly discovered superfamily of bacterial monofunctional PRODHs. The results presented here include production of a monodisperse protein solution through use of the detergent n-octyl β-d-glucopyranoside and the growth of native crystals that diffracted to 2.3 Å resolution at Advanced Light Source beamline 4.2.2. The space group is P2 1 2 1 2 1 , with unit-cell parameters a = 82.2, b = 89.6, c = 94.3 Å. The asymmetric unit is predicted to contain two protein molecules and 46% solvent. Molecular-replacement trials using a fragment of the PRODH domain of the multifunctional Escherichia coli PutA protein as the search model (24% amino-acid sequence identity) did not produce a satisfactory solution. Therefore, the structure of T. thermophilus PRODH will be determined by multiwavelength anomalous dispersion phasing using a selenomethionyl derivative

  17. A green process for the preparation of 11-{4-[2-(2-hydroxyethoxyethyl]-1-piperazinyl}dibenzo[b,f][1,4]thiazepine

    Directory of Open Access Journals (Sweden)

    GANESH D. MAHALE

    2008-04-01

    Full Text Available A green process for the synthesis of 11-{4-[2-(2-hydroxyethoxyethyl]-1-piperazinyl}dibenzo[b,f][1,4]thiazepine by the reaction of 11-(1-piperazinyldibenzo[b,f][1,4]thiazepine or its dihydrochloride salt with 2-(2-chloroethoxyethanol in the presence of an inorganic base and water is reported (conversion 99.9 % in a short time and without any impurities. The metal halides and phase transfer catalyst increase the rate of reaction, especially in water as the solvent.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-08-10

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  20. 5-Isopropylidene-1,3-dithiolo[4,5-d][1,3]dithiole-2-thione

    Directory of Open Access Journals (Sweden)

    Yoshiro Yamashita

    2009-05-01

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

  1. Photo-crosslinkable cyanoacrylate bioadhesive: shrinkage kinetics, dynamic mechanical properties, and biocompatibility of adhesives containing TMPTMA and POSS nanostructures as crosslinking agents.

    Science.gov (United States)

    Ghasaban, S; Atai, M; Imani, M; Zandi, M; Shokrgozar, M-A

    2011-11-01

    The study investigates the photo-polymerization shrinkage behavior, dynamic mechanical properties, and biocompatibility of cyanoacrylate bioadhesives containing POSS nanostructures and TMPTMA as crosslinking agents. Adhesives containing 2-octyl cyanoacrylate (2-OCA) and different percentages of POSS nanostructures and TMPTMA as crosslinking agents were prepared. The 1-phenyl-1, 2-propanedione (PPD) was incorporated as photo-initiator into the adhesive in 1.5, 3, and 4 wt %. The shrinkage strain of the specimens was measured using bonded-disk technique. Shrinkage strain, shrinkage strain rate, maximum and time at maximum shrinkage strain rate were measured and compared. Mechanical properties of the adhesives were also studied using dynamic mechanical thermal analysis (DMTA). Biocompatibility of the adhesives was examined by MTT method. The results showed that shrinkage strain increased with increasing the initiator concentration up to 3 wt % in POSS-containing and 1.5 wt % in TMPTMA-containing specimens and plateaued out at higher concentrations. By increasing the crosslinking agent, shrinkage strain, and shrinkage strain rate increased and the time at maximum shrinkage strain rate decreased. The study indicates that the incorporation of crosslinking agents into the cyanoacrylate adhesives resulted in improved mechanical properties. Preliminary MTT studies also revealed better biocompatibility profile for the adhesives containing crosslinking agents comparing to the neat specimens. Copyright © 2011 Wiley Periodicals, Inc.

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

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2011-02-01

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

  3. IMPAC-2, Dynamic Impact Analysis for 1-D Nonlinear Spring Shipping Container Model

    International Nuclear Information System (INIS)

    Payne, J. B.; Counts, J.

    1980-01-01

    1 - Description of problem or function: IMPAC2 solves the equations of motion for a one-dimensional, lumped-mass, nonlinear spring mathematical container model. The program was designed to analyze the dynamic response of metallic shipping containers impacting an unyielding surface. The container may consist of several hollow concentric cylinders, each of a different material and length. 2 - Method of solution: An iteration technique (Newmark-Beta) is used to solve the equations of motion for displacement, velocity, and acceleration of the masses at each time-step. 3 - Restrictions on the complexity of the problem: The maximum number of masses is 100. The program is written for a maximum of 10 different materials. The first seven have been given the following designations: 1 steel, 2 clad lead, 3 uranium, 4 pine, 5 lead, 6 balsa, 7 marine plywood. Stress-strain characteristics for materials 1, 3, 4, and 6 are approximated by a bilinear curve fit which requires as input the modulus of elasticity, the stress at the intersection of the two lines and the slope of the second line

  4. 3-Cyano-N-methylpyridinium perchlorate

    Directory of Open Access Journals (Sweden)

    Cameron A. McCormick

    2014-07-01

    Full Text Available In the crystal of the title molecular salt, C7H7N2+·ClO4−, the components are linked by C—H...O and C—H...N interactions, generating zigzag chains running parallel to [100].

  5. Uji Aktivitas Antibakteri 1-[(Kuinazolin-4-on-2-ilmetil]piridin-1-ium Bromida dan 2-Bromometilkuinazolin-4-on

    Directory of Open Access Journals (Sweden)

    Hayun

    2014-04-01

    Full Text Available Antibacterial activity tests of quinazolin-4-one derivates: 1-[(6-nitroquinazolin-4-one- 2-ylmethyl]piridin-1-ium bromide (1, 1-[(6-aminoquinazolin-4-on-2-ylmethyl]piridin-1-um bromide (2, 2-bromomethylquinazolin-4-one (3 and 2-bromomethyl-6-nitroquinazolin-4-one (4 with trimethoprim (5 as a positive standard were conducted. The antibacterial activity tests were carried out using disc diffusion method againts E. coli, S. aureus and S. thyposa, and determination of minimum inhibitory concentration (MIC. The results showed that compounds 1 and 2 are inactive as antibacterial, whereas compounds 3 and 4 are active. The activities to E. coli were ¼ times the activity of trimethoprim (MIC: 5 x 102 µg/ml compared to 1.25 x102 µg/ml . The activity to S. typhosa were ½-1 times the activity of trimethoprim (MIC: 2.5 and 1.25x102 µg/ml compared to 1.25x102 µg/ml; but they are not active to S. aureus. Trimethoprim active to S. aureus with MIC: 0.62 x102 µg/ ml.

  6. Crystal structure of bis{μ2-2,2′-[(4,10-dimethyl-1,4,7,10-tetraazacyclododecane-1,7-diylbis(methylene]bis(4-oxo-4H-pyran-3-olato}dicobaltcalcium bis(perchlorate 1.36-hydrate

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    Patrizia Rossi

    2017-12-01

    Full Text Available The title compound, [CaCo2(C22H30N4O62](ClO42·1.36H2O or {Ca[Co(H–2L1]22ClO4·1.36H2O {where L1 is 4,10-bis[(3-hydroxy-4-pyron-2-ylmethyl]-1,7-dimethyl-1,4,7,10-tetraazacyclododecane}, is a trinuclear complex whose asymmetric unit comprises a quarter of the {Ca[Co(H–2L1]2}2+ trinuclear complex, half of a perchlorate ion and 0.34-water molecules. In the neutral [Co(H–2L1] moiety, the cobalt ion is hexacoordinated in a trigonal–prismatic fashion by the surrounding N4O2 donor set. A Ca2+ cation holds together two neutral [Co(H–2L1] moieties and is octacoordinated in a distorted trigonal–dodecahedral fashion by the surrounding O atoms belonging to the deprotonated oxide and carbonyl groups of two [Co(H–2L1] units. The coordination of the CoII cation preorganizes L1 and an electron-rich area forms, which is able to host hard metal ions. The comparison between the present structure and the previously published ones suggests a high versatility of this ligand; indeed, hard metal ions with different nature and dimensions lead to complexes having different stoichiometry (mono- and dinuclear monomers and trinuclear dimers or even a polymeric structure. The heterotrinuclear CoII–CaII–CoII complexes are connected in three dimensions via weak C—H...O hydrogen bonds, which are also responsible for the interactions with the perchlorate anions and the lattice water molecules. The perchlorate anion is disordered about a twofold rotation axis and was refined giving the two positions a fixed occupancy factor of 0.5. The crystal studied was refined as a two-component inversion twin [BASF parameter = 0.14 (4].

  7. Bis(μ-2-carboxymethyl-2-hydroxybutanedioatobis[diaquamanganese(II]–1,2-bis(pyridin-4-ylethene–water (1/1/2

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    In Hong Hwang

    2012-12-01

    Full Text Available The asymmetric unit of the title compound, [Mn2(C6H6O72(H2O4]·C12H10N2·2H2O, contains half of the centrosymmetric Mn complex dimer, half of a 1,2-bis(pyridin-4-ylethene molecule, which lies across an inversion center, and one water molecule. Two citrate ligands bridge two MnII ions, and each MnII atom is coordinated by four O atoms from the citrate ligands (one from hydroxy and three from carboxylate groups and two water O atoms, forming a distorted octahedral environment. In the crystal, O—H...O and O—H...N hydrogen bonds link the centrosymmetric dimers and lattice water molecules into a three-dimensional structure which is further stabilized by intermolecular π–π interactions [centroid–centroid distance = 3.959 (2 Å]. Weak C—H...O hydrogen bonding interactions are also observed.

  8. Anodic oxidation, electro-Fenton and photoelectro-Fenton degradations of pyridinium- and imidazolium-based ionic liquids in waters using a BDD/air-diffusion cell

    International Nuclear Information System (INIS)

    Garcia-Segura, Sergi; Lima, Álvaro Silva; Cavalcanti, Eliane Bezerra; Brillas, Enric

    2016-01-01

    Highlights: • Treatment of 1-butyl-4-methylpyridinium chloride and 1-ethyl-3-methylimidazolium chloride. • Almost total mineralization of both compounds by AO-H_2O_2, EF and PEF at high current density. • Release of NH_4"+ and NO_3"− in different proportion depending on the ionic liquid. • Large decay of initial Cl"− with main formation of ClO_3"− and, in lesser extent, of ClO_4"−. • Detection of primary heteroaromatic products and carboxylic acids generated. - Abstract: The degradation of two representative ionic liquids, 1-butyl-4-methylpyridinium chloride and 1-ethyl-3-methylimidazolium chloride, has been studied in 100 cm"3 of aqueous sulfate medium of pH 3.0 by electrochemical advanced oxidation processes (EAOPs) like anodic oxidation with electrogenerated H_2O_2 (AO-H_2O_2), electro-Fenton (EF) and photoelectro-Fenton (PEF). The electrolytic cell contained a boron-doped diamond (BDD) anode and an air diffusion cathode. The main oxidants were hydroxyl radicals formed at the anode surface from water discharge and in the bulk from Fenton’s reaction between generated H_2O_2 and added Fe"2"+. The solutions of both compounds underwent an almost total mineralization with 97% and 94% of dissolved organic abatement by the most powerful PEF at high current density, being similar and slightly lower for AO-H_2O_2 and EF, respectively. At low current density, the pyridinium-based ionic liquid showed similar mineralization rate by AO-H_2O_2 and PEF, whereas the imidazolium-based ionic liquid was more rapidly degraded in the sequence: AO-H_2O_2 < EF < PEF, where the positive effect of UVA irradiation in PEF was more apparent. The current efficiency decreased gradually with increasing current density in all EAOPs and its value was always superior for the latter compound. The NO_3"− and NH_4"+ concentrations produced in each process were quantified by ion chromatography. This technique confirmed a drastic oxidation of Cl"− contained in the parent

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

    Science.gov (United States)

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

    2009-12-12

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

  10. INVESTIGAREA METODELOR DE SINTEZĂ PENTRU 3-(ANTRACEN-9-IL-1-(4-IZOTIOCIANATOFENIL-PROP-2-EN-1-ONĂ

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    Ana POPUŞOI

    2017-03-01

    Full Text Available Lucrarea prezintă o descriere succintă a izotiocianatochalconelor fluorescente şi redă unele metode de obţinere a lor. În aspect mai detaliat sunt cercetate metodele de obţinere a izotiocianatochalconelor ce conţin fragmentul antracenic. Rezultate bune atestă metoda ce include condensarea 3-(4-acetilfenil-1,1-dimetiltioureei cu antracen-9-carbaldehidă, urmată de eliminarea dimetilaminei din chalconele corespunzătoare la tratare cu anhidridă acetică sau cu clorură de acetil.THE INVESTIGATION OF SYNTHESIS METHODS FOR 3-(ANTHRACEN-9-YL-1-(4-ISOTHIOCYANATOPHENYLPROP-2-EN-1-ONEThe paper presents a review of the isothiocyanatochalcones fluorescents and their methods of synthesis. Various methods were investigated for obtaining anthracene moiety containing isothiocyanatochalcones. Good results give the method which includes condensation of 3-(4-acetylphenyl-1,1-dimethylamine with antracene-9-carbaldehyde flowed by elimination of dimethylamine in the treatment of corresponding chacones with acetyl anhydride or acetyl chloride.

  11. High sensitivity cavity ring down spectroscopy of N_2O near 1.22 µm: (II) "1"4N_2"1"6O line intensity modeling and global fit of "1"4N_2"1"8O line positions

    International Nuclear Information System (INIS)

    Tashkun, S.A.; Perevalov, V.I.; Karlovets, E.V.; Kassi, S.; Campargue, A.

    2016-01-01

    In a recent work (Karlovets et al., 2016 [1]), we reported the measurement and rovibrational assignments of more than 3300 transitions belonging to 64 bands of five nitrous oxide isotopologues ("1"4N_2"1"6O, "1"4N"1"5N"1"6O, "1"5N"1"4N"1"6O, "1"4N_2"1"8O and "1"4N_2"1"7O) in the high sensitivity CRDS spectrum recorded in the 7915–8334 cm"−"1 spectral range. The assignments were performed by comparison with predictions of the effective Hamiltonian models developed for each isotopologue. In the present paper, the large amount of measurements from our previous work mentioned above and literature are gathered to refine the modeling of the nitrous oxide spectrum in two ways: (i) improvement of the intensity modeling for the principal isotopologue, "1"4N_2"1"6O, near 8000 cm"−"1 from a new fit of the relevant effective dipole moment parameters, (ii) global modeling of "1"4N_2"1"8O line positions from a new fit of the parameters of the global effective Hamiltonian using an exhaustive input dataset collected in the literature in the 12–8231 cm"−"1 region. The fitted set of 81 parameters allowed reproducing near 5800 measured line positions with an RMS deviation of 0.0016 cm"−"1. The dimensionless weighted standard deviation of the fit is 1.22. As an illustration of the improvement of the predictive capabilities of the obtained effective Hamiltonian, two new "1"4N_2"1"8O bands could be assigned in the CRDS spectrum in the 7915–8334 cm"−"1 spectral range. A line list at 296 K has been generated in the 0–10,700 cm"−"1 range for "1"4N_2"1"8O in natural abundance with a 10"−"3"0 cm/molecule intensity cutoff. - Highlights: • Line parameters of two new "1"4N_2"1"8O bands centered at 7966 cm"−"1 and at 8214 cm"−"1. • Refined sets of the "1"4N_2"1"6O effective dipole moment parameters for ΔP=13,14 series. • Global modeling of "1"4N_2"1"8O line positions and intensities in the 12–8231 cm"−"1 range. • 5800 observed of "1"4N_2"1"8O line positions

  12. 2-(5,6-Diphenyl-1,2,4-triazin-3-ylaniline

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    Mariusz Mojzych

    2012-12-01

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

  13. Physiological and biochemical responses of wheat (Triticum aestivum L.) seedlings to three imidazolium-based ionic liquids in soil.

    Science.gov (United States)

    Xu, Yaqi; Wang, Jun; Zhu, Lusheng; Du, Zhongkun; Wang, Jinhua; Wei, Kai

    2018-01-01

    Ionic liquids (ILs) are considered environmentally friendly solvents and are widely applied in various fields; however, some researchers have noted the toxicity of ILs to plants cultivated in nutrient solution. To evaluate the toxicities of ILs to wheat seedlings in soil, the natural growth environment of plants, a study was performed using three imidazolium-based ionic liquids with different anions: 1-octyl-3-methylimidazolium chloride ([C 8 mim]Cl), 1-octyl-3-methylimidazolium bromide ([C 8 mim]Br) and 1-octyl-3-methylimidazolium tetrafluoroborate ([C 8 mim]BF 4 ). After 13 d of exposure to these three ILs at 0, 100, 200, 400, 600 and 800 mg kg -1 in brown soil, wheat seedlings were randomly sampled to evaluate growth (shoot length, root length, pigment content and proline content), lipid peroxidation, oxygen species (H 2 O 2 and O 2 - ) and activities of the detoxification enzyme glutathione-s-transferase and other antioxidant enzymes, including superoxide dismutase, catalase and peroxidase. The experimental results showed that all three ILs had inhibitory effects on the growth of wheat seedlings and induced the generation of reactive oxygen species, which indicated that the wheat seedlings suffered oxidative stress. Moreover, antioxidant enzyme activity was enhanced after exposure to [C 8 mim]Cl, [C 8 mim]Br and [C 8 mim]BF 4 , demonstrating that oxidative damage may be the primary underlying mechanism of IL toxicity in wheat. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Anti-natural octyl disaccharide-leprosy IDRI diagnostic (NDO-LID) antibodies as indicators of leprosy reactions and neuritis.

    Science.gov (United States)

    Serrano-Coll, Héctor; Muñoz, Mónica; Camilo Beltrán, Juan; Duthie, Malcolm S; Cardona-Castro, Nora

    2017-03-01

    Leprosy is a complex infectious and neurological disease caused by Mycobacterium leprae. Nerve damage is related to immunological hypersensitivity responses known as leprosy reactions (LRs). Diagnostic tools to predict LRs are not available. We hypothesized that natural octyl disaccharide-leprosy IDRI diagnostic (NDO-LID) would be helpful as an indicator of LRs and neuritis. To assess the utility of NDO-LID in indicating reactions, ELISA were used to detect specific antibodies in serum samples from 80 Colombian leprosy patients (40 with and 40 without history of LRs). Responses were detected using a range of detection reagents detecting IgG, IgM or both isotypes. Patients with a history of LRs had an increased seropositivity rate for anti-NDO-LID antibodies compared to patients without (anti-NDO-LID protein A [p=0.02], IgG anti-NDO-LID [p=0.01] and IgM anti-NDO-LID [p=0.01]). Further analyses of patients with a history of LRs indicated that both seropositivity rate and magnitude of responses were elevated among patients with neuritis versus those without neuritis (anti-NDO-LID protein A [p=0.03], IgG anti-NDO-LID [p=0.001] and IgM anti-NDO-LID [p=0.06]). Our data indicate that testing for serum anti-NDO-LID antibodies can be a useful screen to identify patients at risk of developing LRs and neuritis. © The Author 2017. Published by Oxford University Press on behalf of Royal Society of Tropical Medicine and Hygiene. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  15. Preliminary study of insect attraction by a mixture of semiochemicals containing 1,2,4-Trimethoxybenzene in domestic citric-culture

    Energy Technology Data Exchange (ETDEWEB)

    Alves, Ana Paula L.; CJunior, Jose Augusto B. de; Slana, Glaucia B. A.; Cardoso, Jari N.; Lopes, Rosangela S. C.; Lopes, Claudio C. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Inst. de Quimica. Dept. de Quimica Analitica

    2010-07-01

    In this work we describe a new efficient strategy for the preparation of 1,2,4-trimethoxybenzene (3) in 56% overall yield. The compound 3 was used in a preliminary study of insect attraction by a mixture of semiochemicals called TIV, composed of indol (1), vanillin (2) and 1,2,4-trimethoxybenzene (3), in eight Mc Phail style traps installed at a domestic orchard of citric-culture, containing 120 trees not infected by plagues in Bom Jesus Farm, located next to a patch of the Atlantic Forest, at Silva Jardim, Rio de Janeiro, Brazil. (author)

  16. Photostabilization studies of antihypertensive 1,4-dihydropyridines using polymeric containers.

    Science.gov (United States)

    De Luca, Michele; Ioele, Giuseppina; Spatari, Claudia; Ragno, Gaetano

    2016-05-30

    1,4-dihydropyridine antihypertensives (DHPs) are almost all dispensed in solid pharmaceutical formulations for their easy lability when exposed to light. This paper reports a study on the photoprotective effect of containers in different glassy or polymeric matrices with regard to four known DHPs when in solutions. The samples were subjected to forced degradation by means of a Xenon lamp, in accordance with the international rules on drug stability evaluation. The simultaneous determination of the drugs and their photoproducts was carried out by applying the multivariate curve resolution (MCR) methodology to the spectral data recorded along the irradiation test. This technique was able to determine the kinetic parameters and resolve the spectra of the photoproducts. The time required to reduce by 10% the concentration of the drug (t0.1) was adopted as a criterion to compare the protective ability of the containers. A significant photoprotection for all drugs tested was obtained by the use of polyethylene terephthalate (PET) containers. The best result was achieved for the felodipine solution in blue PET transparent bottle of 0.6mm thickness, reaching an almost complete stabilization up to six hours under stressing irradiation. In contrast, the glass containers, whether or not coloured, did not provide a satisfactory photoprotection of the drugs, showing in any case t0.1 values under 24min. These results can be a good opportunity to design new photoprotective pharmaceutical packaging for DHPs in liquid dosage form. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. (2E-1-(3-Chlorophenyl-3-(4-chlorophenylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    Jerry P. Jasinski

    2009-11-01

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

  18. Immobilization of Pseudomonas fluorescens lipase on hydrophobic supports and application in biodiesel synthesis by transesterification of vegetable oils in solvent-free systems.

    Science.gov (United States)

    Lima, Lionete N; Oliveira, Gladson C; Rojas, Mayerlenis J; Castro, Heizir F; Da Rós, Patrícia C M; Mendes, Adriano A; Giordano, Raquel L C; Tardioli, Paulo W

    2015-04-01

    This work describes the preparation of biocatalysts for ethanolysis of soybean and babassu oils in solvent-free systems. Polystyrene, Amberlite (XAD-7HP), and octyl-silica were tested as supports for the immobilization of Pseudomonas fluorescens lipase (PFL). The use of octyl-silica resulted in a biocatalyst with high values of hydrolytic activity (650.0 ± 15.5 IU/g), immobilization yield (91.3 ± 0.3 %), and recovered activity (82.1 ± 1.5 %). PFL immobilized on octyl-silica was around 12-fold more stable than soluble PFL, at 45 °C and pH 8.0, in the presence of ethanol at 36 % (v/v). The biocatalyst provided high vegetable oil transesterification yields of around 97.5 % after 24 h of reaction using babassu oil and around 80 % after 48 h of reaction using soybean oil. The PFL-octyl-silica biocatalyst retained around 90 % of its initial activity after five cycles of transesterification of soybean oil. Octyl-silica is a promising support that can be used to immobilize PFL for subsequent application in biodiesel synthesis.

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

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    Gabriella Cavallo

    2014-01-01

    Full Text Available The title compound, C25H18F4P+·Br−·C2F4I2, is a 1:1 co-crystal of triphenyl(2,3,5,6-tetrafluorobenzylphosphonium (TTPB bromide and 1,1,2,2-tetrafluoro-1,2-diiodoethane (TFDIE. The crystal structure consists of a framework of TTPB cations held together by C—H...Br interactions. In this framework, infinite channels along [100] are filled by TFDIE molecules held together in infinite ribbons by short F...F [2.863 (22.901 (2Å] interactions. The structure contains halogen bonds (XB and hydrogen bonds (HB in the bromide coordination sphere. TFDIE functions as a monodentate XB donor as only one I atom is linked to the Br− anion and forms a short and directional interaction [I...Br− 3.1798 (7 Å and C—I...Br− 177.76 (5°]. The coordination sphere of the bromide anion is completed by two short HBs of about 2.8 Å (for H...Br with the acidic methylene H atoms and two longer HBs of about 3.0 Å with H atoms of the phenyl rings. Surprisingly neither the second iodine atom of TFDIE nor the H atom on the tetrafluorophenyl group make any short contacts.

  20. N,N'-di-(m-methylphenyi)-3,6-dimethyl-1,4-dihydro-1,2,4,5-tetrazine-1,4-dicarboamide (ZGDHu-1) suppresses the proliferation of PANC-1 pancreatic cancer cells via apoptosis and G2/M cell cycle arrest.

    Science.gov (United States)

    Chen, Su-Feng; Xia, Jun; Lv, Ya-Ping; Liu, Jin-Lin; Li, Wan-Xiang; Yu, Xi-Ping; Hu, Wei-Xiao; Zhou, Yong-Lie

    2015-04-01

    Pancreatic cancer is one of the human gastrointestinal malignancies with a high mortality and poor prognosis. Approximately eighty percent of patients are diagnosed with unresectable or metastatic disease. Thus, development of novel chemicals in the treatment of pancreatic cancer is imperative. This study aimed to investigate the anticancer effects of N,N'-di-(m-methylphenyi)-3,6-dimethyl-1,4-dihydro-1,2,4,5-tetrazine-1,4-dicarboamide (ZGDHu-1), a new tetrazine derivative, on the PANC-1 pancreatic cancer cell line and clarify the underlying molecular mechanism. Using an MTT assay, we found that ZGDHu-1 significantly suppressed the proliferation of PANC-1 cells in a time- and dose-dependent manner. Moreover, according to the morphological and flow cytometric analysis, the results indicated that ZGDHu-1 induced PANC-1 cell apoptosis and G2/M cell cycle arrest in a dose-dependent manner. In the western blot analysis, expression of the pro-apoptotic Bax gene was upregulated while the anti-apoptotic Bcl-2 gene was downregulated following treatment with ZGDHu-1. ZGDHu-1 also activated pro-caspase-3 and PARP and increased the expression of NF-κB inhibitor IκB. Furthermore, the expression levels of G2/M regulatory molecules such as cyclin B1 and cdc2 were decreased while that of Chk1 was increased. These results suggested that ZGDHu-1 suppressed the proliferation of pancreatic cancer cells, rendering it a potential therapeutic drug for the treatment of pancreatic cancer.

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

    Directory of Open Access Journals (Sweden)

    Tilal Elsaman

    2013-01-01

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

  2. Synthesis, characterization, thermal properties and theoretical investigation on Bis(guanidinium) 4,4‧- Azo-1H-1,2,4-triazol-5-one

    Science.gov (United States)

    Cao, Wen-li; Guo, Jia-jia; Chen, Xiang; Ding, Zi-mei; Xu, Kang-zhen; Song, Ji-rong; Fan, An; Huang, Jie

    2017-11-01

    Bis(guanidinium) 4,4‧-Azo-1H-1,2,4-triazol-5-one [G2(ZTO)] was synthesized and characterized by X-ray single crystal diffraction, elemental analyzer and Fourier Transform Infrared (FT-IR) spectrometer. The result from X-ray single crystal diffraction indicates that G2(ZTO) crystallizes in the monoclinic space group P2(1)/c with parameters of a = 4.779(2) Å, b = 9.081(4) Å, c = 14.676(6) Å, α = 90.00°, β = 92.43(7)°, γ = 90.00°, V = 636.4(5) Å3, Z = 2, μ(Mo Kα) = 0.131, F(000) = 328, S = 1.071, Dc = 1.640 g·cm-3, R1 = 0.0510 and wR2 = 0.1389. Interestingly enough, its structure does not contain crystallization water, which is a unique characteristic in this material. Besides, the molecular geometry of the compound was optimized by using Density Functional Theory (DFT) method at B3LYP/6-31G (d, p) level in the ground state, revealing that the obtained geometric parameters are in accordance with the X-ray result of the structure. The experimental vibrational spectrum was compared with the calculated spectrum. Besides, molecular electrostatic potential (MEP) of G2(ZTO) was computed with the same method in gas phase, theoretically. The thermal properties of this compound were investigated by DSC, TG/DTG and micro-DSC methods. The results manifest that its thermal behavior can be divided into two main decomposition stages, the first intense decomposition peak temperature is 248.11 °C at the heating rate of 10 °C·min-1, which is higher than that of RDX (219 °C) but slightly lower than that of G(ZTO)·H2O (252.08 °C). The constant-volume combustion heat (ΔcU) of G2(ZTO), G(ZTO)·H2O and ZTO were determined and then the enthalpy of formation were calculated. The results show that G2(ZTO) possesses the highest standard molar enthalpy of formation, which may be explained by the fact that G2(ZTO) contains no water and possesses the highest nitrogen content in all guanidine salts. Moreover, the apparent activation energy (E), thermal stability and safety

  3. Separation of toluene from n-heptane by liquid–liquid extraction using binary mixtures of [bpy][BF4] and [4bmpy][Tf2N] ionic liquids as solvent

    International Nuclear Information System (INIS)

    García, Silvia; Larriba, Marcos; García, Julián; Torrecilla, José S.; Rodríguez, Francisco

    2012-01-01

    Highlights: ► Binary mixtures of ionic liquids as extraction solvents of aromatics. ► [4bmpy][Tf 2 N] shows higher capacity but lower selectivity than sulfolane. ► [bpy][BF 4 ] shows lower capacity but higher selectivity than sulfolane. ► Mixed {[4bmpy][Tf 2 N] + [bpy][BF 4 ]} improves both extractive properties. - Abstract: The use of binary mixture of ionic liquids N-butylpyridinium tetrafluoroborate ([bpy][BF 4 ]), and 1-butyl-4-methylpyridinium bis(trifluoromethylsulfonyl)imide ([4bmpy][Tf 2 N]) in the liquid–liquid extraction of toluene from n-heptane has been investigated at 313.2 K and atmospheric pressure. The experimental capacity of extraction and selectivity for this binary mixture has proved to be intermediate to those corresponding to the pure ionic liquids, and they can be predicted using a logarithmic–linear model of solubility. Furthermore, the results showed that the use of binary mixture of {[bpy][BF 4 ] + [4bmpy][Tf 2 N]} at a mole solvent composition around 0.7 for [bpy][BF 4 ] improves both the capacity of extraction of toluene and the selectivity with respect to those of sulfolane, the organic solvent taken as a benchmark. Thus, this mixed ionic liquid could be likely to be used in the extraction of aromatic from aliphatic in replacement to sulfolane.

  4. 4-(4-Octyloxybenzoyloxybenzoic acid

    Directory of Open Access Journals (Sweden)

    Shahid Hameed

    2009-02-01

    Full Text Available The title compound, C22H26O5, is an important intermediate for the synthesis of side-chain ligands for polymeric liquid crystals. The octyl group is coplanar with the central C6O moiety, where the maximum deviation of a C atom in the octyl group from the C6O plane is 0.161 (5 Å. The crystal structure is stabilized by intermolecular O—H...O hydrogen bonds.

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

    International Nuclear Information System (INIS)

    Van Ree, T.

    1989-01-01

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

  6. Effect of HTGR helium on fatigue and creep properties of 2 1/4Cr-1Mo steel

    International Nuclear Information System (INIS)

    Kurumaji, T.; Yamazaki, H.; Kudo, A.

    1982-01-01

    Low cycle fatigue and creep tests have been carried out on 2 1/4Cr-1Mo steel (candidate steel for VHTR reactor pressure vessel) in helium environment containing 200 approx. 300 μatm of H 2 , 100 approx. 150 μatm CO, 7 approx. 10 μatm CH 4 , 7 approx. 10 μatm CO 2 and 1 μatm H 2 O (JAERI B Helium). Fatigue life in helium environment was longer than that in air at 450 0 C. This results can be explained by supposing that oxidation at the crack tip causes the wedge effect to promote crack propagation in air. On the otherhand, creep rupture strength showed no significant difference in both helium and air. Equivalent creep rupture strength in both helium and air may be due to the fact that detrimental internal oxidation and carburization or decarburization hardly occur at 400 approx. 450 0 C

  7. Carboranyl tetrahydroisoquinolines. Synthesis and the X-ray structural study of 1-(o-Carboran-1-ylmethyl)-1,2,3,4-Tetrahydroisoquinolines

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jong Dae; Kang, Sang Ook [Korea University, Dept. of Chemistry, Chung-nam (Korea); Lee, Chai-Ho [Wonkwang Univ., Dept. of Chemistry, Jeonbuk (Korea); Lee, Seung-Hoon [National Cancer Center, Kyungi-do (Korea); Lim, Sang-Moo [Korea Cancer Center Hospital, Seoul (Korea); Cho, Sungil [Seoul City Univ., Dept. of Chemical Engineering, Seoul (Korea)

    2001-11-01

    Synthesis of the first fully characterized boronated tetrahydroisoquinolines is reported. Thus, tetrahydroisoquinolines containing 1-(0-carboran-1-ylmethyl)-1,2,3,4-tetrahydroisoquinolines have been synthesized from the corresponding arylethylamines to provide carboranes attached to functional group capable of being covalently incorporated into structures of potential use in boron neutron capture therapy (BNCT). The carboranyl functionalities were attached at the 1-position of the tetrahydroisoquinoline molecule. Experimental details and analytical data leading to the identification of the reported compounds are provided. Additionally, the X-ray diffraction structure of 9b is reported. (author)

  8. Kinetic studies of Chromobacterium viscosum lipase in AOT water in oil microemulsions and gelatin microemulsion-based organogels.

    Science.gov (United States)

    Jenta, T R; Batts, G; Rees, G D; Robinson, B H

    1997-06-05

    Kinetic studies have shown that octyl decanoate synthesis by Chromobacterium viscosum (CV) lipase in sodium bis-2-(ethylhexyl) sulfosuccinate (AOT) water in oil (w/o) microemulsions occurs via the nonsequential (ping-pong) bi bi mechanism. There was evidence of single substrate inhibition by decanoic acid at high concentrations. Initial rate data yielded estimates for acid and alcohol Michaelis constants of ca. 10(-1) mol dm(-3) and a maximum rate under saturation conditions of ca. 10(-3) mol dm(-3) s(-1) for a lipase concentration of 0.36 mg cm(-3). CV lipase immobilized in AOT microemulsion-based organogels (MBGs) was also found to catalyze the synthesis of octyl decanoate according to the ping-pong bi bi mechanism. Reaction rates were similar in the free and immobilized systems under comparable conditions. Initial rates at saturating (but noninhibiting) substrate concentrations were first order with respect to CV lipase concentration in both w/o microemulsions and the MBG/oil systems. Gradients yielded an apparent k(cat) = 4.4 x 10(-4) mol g(-1) s(-1) in the case of w/o microemulsions, and 6.1 x 10(-4) mol g(-1) s(-1) for CV lipase immobilized in the MBGs. A third system comprising w/o microemulsions containing substrates and gelatin at concentrations comparable to those employed in the MBG formulations, provided a useful link between the conventional liquid microemulsion medium and the solid organogels. The nongelation of these intermediate systems stems from the early inclusion of substrate during a modified preparative protocol. The presence of substrate appears to prevent the development of a percolated microstructure that is thought to be a prerequisite for MBG formation. FT-NMR was employed as a semicontinuous in situ assay procedure. The apparent activity expressed by CV lipase in compositionally equivalent liquid and solid phase gelatin-containing systems was similar. An apparent activation energy of 24 +/- 2 kJ mol(-1) was determined by (1)H-NMR for

  9. Poly[[sesqui[mu2-1,4-bis(imidazol-1-ylmethyl)benzene-kappa(2)N:N'](carbonato-kappa(2)O,O')copper(II)] 1,4-bis(imidazol-1-ylmethyl)benzene hemisolvate pentahydrate].

    Science.gov (United States)

    Dai, Yu-Mei; Tang, En; Huang, Jin-Feng; Yang, Qiu-Yan

    2008-10-01

    The asymmetric unit of the title compound, {[Cu(CO(3))(C(14)H(14)N(4))(1.5)] x 0.5 C(14)H(14)N(4) x 5 H(2)O}(n), contains one Cu(II) cation in a slightly distorted square-pyramidal coordination environment, one CO(3)(2-) anion, one full and two half 1,4-bis(imidazol-1-ylmethyl)benzene (bix) ligands, one half-molecule of which is uncoordinated, and five uncoordinated water molecules. One of the coordinated bix ligands and the uncoordinated bix molecule are situated about centers of symmetry, located at the centers of the benzene rings. The coordinated bix ligands link the copper(II) ions into a [Cu(bix)(1.5)](n) molecular ladder. These molecular ladders do not form interpenetrated ladders but are arranged in an ABAB parallel terrace, i.e. with the ladders arranged one above another, with sequence A translated with respect to B by 8 A. To best of our knowledge, this arrangement has not been observed in any of the molecular ladder frameworks synthesized to date. The coordination environment of the Cu(II) atom is completed by two O atoms of the CO(3)(2-) anion. The framework is further strengthened by extensive O-H...O and O-H...N hydrogen bonds involving the water molecules, the O atoms of the CO(3)(2-) anion and the N atoms of the bix ligands. This study describes the first example of a molecular ladder coordination polymer based on bix and therefore demonstrates further the usefulness of bix as a versatile multidentate ligand for constructing coordination polymers with interesting architectures.

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

    Directory of Open Access Journals (Sweden)

    D. S. Ismailova

    2014-03-01

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

  11. Discovery and biological evaluation of some (1H-1,2,3-triazol-4-yl)methoxybenzaldehyde derivatives containing an anthraquinone moiety as potent xanthine oxidase inhibitors.

    Science.gov (United States)

    Zhang, Ting-Jian; Li, Song-Ye; Yuan, Wei-Yan; Wu, Qing-Xia; Wang, Lin; Yang, Su; Sun, Qi; Meng, Fan-Hao

    2017-02-15

    A series of (1H-1,2,3-triazol-4-yl)methoxybenzaldehyde derivatives containing an anthraquinone moiety were synthesized and identified as novel xanthine oxidase inhibitors. Among them, the most promising compounds 1h and 1k were obtained with IC 50 values of 0.6μM and 0.8μM, respectively, which were more than 10-fold potent compared with allopurinol. The Lineweaver-Burk plot revealed that compound 1h acted as a mixed-type xanthine oxidase inhibitor. SAR analysis showed that the benzaldehyde moiety played a more important role than the anthraquinone moiety for inhibition potency. The basis of significant inhibition of xanthine oxidase by 1h was rationalized by molecular modeling studies. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Biochemical toxicity and DNA damage of imidazolium-based ionic liquid with different anions in soil on Vicia faba seedlings.

    Science.gov (United States)

    Liu, Tong; Zhu, Lusheng; Wang, Jinhua; Wang, Jun; Zhang, Jun; Sun, Xi; Zhang, Cheng

    2015-12-17

    In the present study, the toxic effects of 1-octyl-3-methylimidazolium chloride ([Omim]Cl), 1-octyl-3-methylimidazolium bromide ([Omim]Br) and 1-octyl-3-methylimidazolium tetrafluoroborate ([Omim]BF4) in soil on Vicia faba (V. faba) seedlings at 0, 100, 200, 400, 600 and 800 mg kg(-1) were assessed for the first time at the cellular and molecular level. Moreover, the toxicity of these three ionic liquids (ILs) was evaluated, and the influence of anions on the toxicity of the ILs was assessed. The results showed that even at 100 mg kg(-1), the growth of V. faba seedlings was inhibited after exposure to the three ILs, and the inhibitory effect was enhanced with increasing concentrations of the three ILs. The level of reactive oxygen species (ROS) was increased after exposure to the three ILs, which resulted in lipid peroxidation, DNA damage and oxidative damage in the cells of the V. faba seedlings. In addition, the anion structure could influence the toxicity of ILs, and toxicity of the three tested ILs decreased in the following order: [Omim]BF4 > [Omim]Br > [Omim]Cl. Moreover, oxidative damage is the primary mechanism by which ILs exert toxic effects on crops, and ILs could reduce the agricultural productivity.

  13. Novel 3-Amino-6-chloro-7-(azol-2 or 5-yl-1,1-dioxo-1,4,2-benzodithiazine Derivatives with Anticancer Activity: Synthesis and QSAR Study

    Directory of Open Access Journals (Sweden)

    Aneta Pogorzelska

    2015-12-01

    Full Text Available A series of new 3-amino-6-chloro-7-(azol-2 or 5-yl-1,1-dioxo-1,4,2-benzodithiazine derivatives 5a–j have been synthesized and evaluated in vitro for their antiproliferative activity at the U.S. National Cancer Institute. The most active compound 5h showed significant cytotoxic effects against ovarian (OVCAR-3 and breast (MDA-MB-468 cancer (10% and 47% cancer cell death, respectively as well as a good selectivity toward prostate (DU-145, colon (SW-620 and renal (TK-10 cancer cell lines. To obtain a deeper insight into the structure-activity relationships of the new compounds 5a–j QSAR studies have been applied. Theoretical calculations allowed the identification of molecular descriptors belonging to the RDF (RDF055p and RDF145m in the MOLT-4 and UO-31 QSAR models, respectively and 3D-MorSE (Mor32m and Mor16e for MOLT-4 and UO-31 QSAR models descriptor classes. Based on these data, QSAR models with good robustness and predictive ability have been obtained.

  14. MABGEL 1: first phase 1 trial of the anti-HIV-1 monoclonal antibodies 2F5, 4E10 and 2G12 as a vaginal microbicide.

    Directory of Open Access Journals (Sweden)

    Georgina C Morris

    Full Text Available BACKGROUND: Monoclonal antibodies (mAbs which potently neutralize a broad range of HIV isolates are potential microbicide candidates. To date, topical application of mAbs in humans and their stability in vaginal secretions has not been studied. OBJECTIVES: To assess the pharmacokinetics and safety of the mAbs 2F5, 4E10 and 2G12 when applied vaginally in women. DESIGN: A randomized, double-blind, placebo-controlled phase 1 trial. METHODS: Twenty-eight healthy, sexually abstinent women administered 2.5 g of gel daily for 12 days containing either 10 or 20 mg/g of each mAb (MABGEL or placebo. Main clinical evaluations and sampling occurred at baseline, 1, 8, and 24 hours post-1st dose and 12 and 36 hours post-12th dose. RESULTS: After adjustment for dilution factors, median levels of 2F5, 4E10 and 2G12 in vaginal secretions at 1 hour post high-dose MABGEL were 7.74, 5.28 and 7.48 mg/ml respectively. Levels of 2F5 and 4E10 declined exponentially thereafter with similar estimated half-lives (4.6 and 4.3 hours. In contrast, 2G12 levels declined more rapidly in the first 8 hours, with an estimated half-life of 1.4 hours during this period. There was no evidence of systemic absorption. There were no significant differences in local or systemic adverse event rates or vaginal flora changes (by qPCR between active and placebo gel arms. Whilst at least 1 adverse event was recorded in 96% of participants, 95% were mild and none were serious. CONCLUSIONS: Vaginal application of 50 mg of each mAb daily was safe over a 12 day period. Median mAb concentrations detected at 8 hours post dose were potentially sufficient to block HIV transmission.2G12 exhibited more rapid elimination from the human vagina than 4E10 and 2F5, likely due to poor stability of 2G12 in acidic human vaginal secretions. Further research is needed to develop mAb-based vaginal microbicides and delivery systems. TRIAL REGISTRATION: ISRCTN 64808733 UK CRN Portfolio 6470.

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

    International Nuclear Information System (INIS)

    Zolotarev, K.I.

    2014-10-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-12-01

    Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space group1' mime-subtype='gif' type='simple'/>$P\\bar 1$,Z= 2, with the unit-cell parametersa= 6.37433(9),b= 11.3641(2),c= 14.09115(19) Å,α= 80.1740(8)°,β= 85.1164(8)°,γ= 80.9831(10)°,V= 991.55(3) Å3of compound (1) anda= 6.53736(6),b= 11.55725(15),c= 14.01373(13) Å,α= 80.3323(7)°,β= 84.8939(6)°,γ= 79.3954(8)°,V= 1024.08(2) Å3of compound (2). Structural analyses reveal that the title compounds are isostructural.

  17. New coordination polymers from 1D chain, 2D layer to 3D framework constructed from 1,2-phenylenediacetic acid and 1,3-bis(4-pyridyl)propane flexible ligands

    International Nuclear Information System (INIS)

    Xin Lingyun; Liu Guangzhen; Wang Liya

    2011-01-01

    The hydrothermal reactions of Cd, Zn, or Cu(II) acetate salts with H 2 PHDA and BPP flexible ligands afford three new coordination polymers, including [Cd(PHDA)(BPP)(H 2 O)] n (1), [Zn(PHDA)(BPP)] n (2), and [Cu 2 (PHDA) 2 (BPP)] n (3) (H 2 PHDA=1,2-phenylenediacetic acid, BPP=1,3-bis(4-pyridyl)propane). The single-crystal X-ray diffractions reveal that all three complexes feature various metal carboxylate subunits extended further by the BPP ligands to form a diverse range of structures, displaying a remarked structural sensitivity to metal(II) cation. Complex 1 containing PHDA-bridged binuclear cadmium generates 1D double-stranded chain, complex 2 results in 2D→2D interpenetrated (4,4) grids, and complex 3 displays a 3D self-penetrated framework with 4 8 6 6 8 rob topology. In addition, fluorescent analyses show that both 1 and 2 exhibit intense blue-violet photoluminescence in the solid state. - Graphical Abstract: We show diverse supramolecular frameworks based on the same ligands (PHDA and BPP) and different metal acetate salts including 1D double-stranded chain, 2D → 2D twofold interpenetrated layer, and 3D self-penetration networks. Highlights: → Three metal(II = 2 /* ROMAN ) coordination polymers were synthesized using H 2 PHDA and BPP. → The diversity of structures show a remarked sensitivity to metal(II) center. → Complexes show the enhancement of fluorescence compared to that of free ligand.

  18. Structural annotation of Beta-1,4-N-acetyl galactosaminyltransferase 1 (B4GALNT1) causing Hereditary Spastic Paraplegia 26.

    Science.gov (United States)

    Dad, Rubina; Malik, Uzma; Javed, Aneela; Minassian, Berge A; Hassan, Muhammad Jawad

    2017-08-30

    Beta-1,4-N-acetyl galactosaminyltransferase 1, B4GALNT1, is a GM2/GD2 synthase, involved in the expression of glycosphingolipids (GSLs) containing sialic acid. Mutations in the gene B4GALNT1 cause Hereditary Spastic Paraplegia 26 (HSP26). In present study we have made attempt to predict the potential structural of the human B4GALNT1 protein. The results illustrated that the amino acid sequences of B4GALNT1 are not 100% conserved among selected twenty species. One signal peptide and one transmembrane domain predicted in human wild type B4GALNT1 protein with aliphatic index of 92.76 and theoretical (iso-electric point) pI of 8.93. It was a kind of unstable protein with Grand average of hydropathicity (GRAVY) of -0.127. Various post-translational modifications were also predicted to exist in B4GALNT1 and predicted to interact with different proteins including ST8SIA5, SLC33A1, GLB1 and others. In the final round, reported missense mutations have shown the further decrease in stability of the protein. This in-silico analysis of B4GALNT1 protein will provide the basis for the further studies on structural variations and biological pathways involving B4GALNT1 in the HSP26. Copyright © 2017. Published by Elsevier B.V.

  19. Copper(II) complexes with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid: Syntheses, crystal structures and antifungal activities

    International Nuclear Information System (INIS)

    Xiong, Pingping; Li, Jie; Bu, Huaiyu; Wei, Qing; Zhang, Ruolin; Chen, Sanping

    2014-01-01

    Reaction of Cu(II) with an asymmetric semi-rigid organic ligand 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid (HL), yielded five compounds, [Cu 0.5 L] n (1), [Cu(HL) 2 Cl 2 ] n (2), [Cu(HL) 2 Cl 2 (H 2 O)] (3), [Cu(L) 2 (H 2 O)] n (4) and [Cu(L)(phen)(HCO 2 )] n (5), which have been fully characterized by infrared spectroscopy, elemental analysis, and single-crystal X-ray diffraction. As for compounds 1, 2 and 5, Cu(II) is bridged through HL, Cl - , and formic acid, respectively, featuring 1D chain-structure. In compound 3, Cu(II) with hexahedral coordination sphere is assembled through hydrogen-bonding into 3D supramolecular framework. In compound 4, 1D chain units –Cu–O–Cu–O– are ligand-bridged into a 3D network. All compounds were tested on fungi (Fusarium graminearum, Altemaria solani, Macrophoma kawatsukai, Alternaria alternata and Colletotrichum gloeosporioides). Compound 1 exhibits a better antifungal effect compared to other compounds. An effect of structure on the antifungal activity has also been correlated. - Graphical abstract: Copper(II) compounds with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid, were prepared, structurally characterized and investigated for antifungal activity. - Highlights: • The title compounds formed by thermodynamics and thermokinetics. • The five compounds show higher inhibition percentage than reactants. • The structure effect on the antifungal activity

  20. (E-2-[4-(Diethylaminostyryl]-1-methylquinolin-1-ium 4-chlorobenzenesulfonate monohydrate

    Directory of Open Access Journals (Sweden)

    Suchada Chantrapromma

    2014-04-01

    Full Text Available The asymmetric unit of the title hydrated salt, C22H25N2+·C6H4ClO3S−·H2O, comprises two 2-[4-(diethylaminostyryl]-1-methylquinolin-1-ium cations, two 4-chlorobenzenesulfonate anions and two solvent water molecules. One ethyl group of both cations displays disorder over two positions in a 0.659 (2:0.341 (2 ratio in one molecule and in a 0.501 (2:0.499 (2 ratio in the other. The sulfonate group of one anion is also disordered over two positions in a 0.893 (7:0.107 (7 ratio. The dihedral angle between the mean plane of the quinolinium ring system and that of benzene ring is 10.57 (18° in one cation and 14.4 (2° in the other. In the crystal, cations, anions and water molecules are linked into chains along the [010] direction by O—H...Osulfonate hydrogen bonds, together with weak C—H...Osulfonate and C—H...Cl interactions. The cations are stacked by π–π interactions, with centroid–centroid distances in the range 3.675 (24.162 (3 Å.

  1. Polyethers containing 4-(carbazol-2-yl)-7-arylbenzo[c]-1,2,5-thiadiazole chromophores as solution processed materials for hole transporting layers of OLEDs

    Science.gov (United States)

    Krucaite, G.; Tavgeniene, D.; Xie, Z.; Lin, X.; Zhang, B.; Grigalevicius, S.

    2018-02-01

    Two polyethers containing electroactive pendent 4-(carbazol-2-yl)-7-arylbenzo[c]-1,2,5-thiadiazole moieties have been synthesized by the multi-step synthetic route. Full characterization of their structures is presented. The polymers represent derivatives of very high thermal stability with initial thermal degradation temperatures of 425 °C and 431 °C. Glass transition temperatures of the amorphous materials were also very high and reached values of 154 °C and 163 °C. The electron photoemission spectra of thin layers of the polymers showed ionization potentials of 5.84 eV and 5.93 eV. Hole-transporting properties of the polymeric materials were tested in the structures of organic light emitting diodes with Alq3 as the green emitter and electron transporting material. An electroluminescent device containing hole-transporting layer (HTL) of the polymer with electroactive 4-carbazolyl-7-phenylbenzo[c]-1,2,5-thiadiazole moieties exhibited turn on voltage of 6.2 V, maximum photometric efficiency of 2.5 cd/A and maximum brightness exceeding 300 cd/m2. The device containing HTL of the polymer with 4-carbazolyl-7-(1-naphtyl)benzo[c]-1,2,5-thiadiazole moieties demonstrated turn on voltage of 5.2 V, maximum photometric efficiency of 1.6 cd/A and maximum brightness exceeding 1500 cd/m2. The efficiencies were about 30-90% higher than that of the device containing widely used hole transporting layers of poly(9-vinylcarbazole).

  2. Fragrance material review on 1-(5,5-dimethylcyclohexen-1-yl)pent-4-en-1-one.

    Science.gov (United States)

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

    2013-12-01

    A toxicologic and dermatologic review of 1-(5,5-dimethylcyclohexen-1-yl)pent-4-en-1-one when used as a fragrance ingredient is presented. 1-(5,5-Dimethylcyclohexen-1-yl)pent-4-en-1-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all published and unpublished toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 1-(5,5-dimethylcyclohexen-1-yl)pent-4-en-1-one were evaluated then summarized and includes physical properties, acute toxicity, skin irritation, mucous membrane (eye) irritation, skin sensitization, and photoallergy data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones When Used as Fragrance Ingredients (submitted for publication)) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

  3. Chelate-size effects on the structures, chemical behavior, properties, and catalytic activity of the new palladium(II)-allyl complexes [Pd(eta(3)-1-R-1-C3H4){FcCH=N-CH2-(CH2)(n)-NMe2}][PF6] {Fc = (eta(5)-C5H5)Fe(eta(5)-C5H4), n=2 or 1, and R-1 = h or ph}

    NARCIS (Netherlands)

    Pérez, S.; López, C.; Bosque, R.; Solans, X.; Font-Bardía, M.; Roig, A.; Molins, E.; van Leeuwen, P.W.N.M.; van Strijdonck, G.P.F.; Freixa, Z.

    2008-01-01

    The synthesis, X-ray crystal structures, and the study of the solution behavior of the palladium(II) allyl complexes [Pd(eta(3)-1R(1)-C3H4){FcCH=N-CH2-(CH2)(n)-NMe2}][PF6] {with Fc = (eta(5)-C5H5)Fe(eta(5)-C5H4), R-1 = H, and n = 2 (4) or 1 (5) or R-1 = Ph and n = 2 (6) or 1 (7)} are described. The

  4. Effects of gamma-irradiation of plastics on migration of constituents into test foods

    International Nuclear Information System (INIS)

    Figge, K.; Freytag, W.

    1977-01-01

    Test films prepared from polyethylene (LD- and HD-PE), polypropylene (PP), polystyrene (St- and HI-PS) and polyvinylchloride (rigid PVC) compositions under addition of 2,6-di-tert-butyl-4-methyl[ 14 C]-phenol(I), 3-(3,5-di-tert-butyl -4-hydroxyphenyl)- stearyl-propionate[3- 14 C] (II), n-butyl-stearate[1- 14 C] (III) di-n-octyl[1- 14 C]-tin-2 -ethyl-hexyl-di-thioglycolate inclusive of the corresponding mono-n-octyl[1- 14 C]-tin compound (IV-Oc), di-n-octyl-tin-2-ethylhexyl -di-thioglycolate[2- 14 C] inclusive of the corresponding 2-ethylhexyl-tri -thioglycolate[2- 14 C] (IV-S) or of stearyl alcohol [1- 14 C] (V) respectively, were sterilized in a 60 Co irradiation unit with a radiation dosage of 2,5 Mrad. Then, the irradiated films as well as non-treated reference films were kept in one-sided contact with the test foodstuffs 'dist. Water' and HB 307 (test fat) for 10 days at 40 0 C. Under these conditions the additives I and II migrated from the PP, HD-PE and LD-PE test films into the test fat HB 307 in amounts of 10 to 50%. Migration into distilled water was only 0.05 to 4.6%. The migration of the additives I and II from the irradiated polyolefin test films into the test fat HB 307 was by 8 to 38% lower than that from the corresponding non-irradiated films. In contrast to this, both additives migrated distinctly more strongly from the irradiated polyolefin test films into distilled water, i.e. 1.9 to 8.7 times stronger than from the non-irradiated films. The migration of the additives I to V from the HI-PS St-PS and rigid PVC test films into the two test foodstuffs was very low, in most cases below 0.1%. Generally lower amounts of additive migrated from the irradiated films than from the non-irradiated samples. (orig.) [de

  5. Assessment of a gel-type chelating preparation containing 1-hydroxyethylidene-1, 1-bisphosphonate.

    Science.gov (United States)

    Girard, S; Paqué, F; Badertscher, M; Sener, B; Zehnder, M

    2005-11-01

    To test an aqueous gel containing 1-hydroxyethylidene-1, 1-bisphosphonate (HEBP) regarding its interactions with sodium hypochlorite, its calcium binding capacity, and its potential in preventing the formation of a smear layer when used in conjunction with rotary root canal preparation. The experimental aqueous gel consisted of (w/v) 2% alginate, 3% aerosil, 10% Tween 80 and 18% HEBP. Interactions of gel components with hypochlorite were assessed using iodometric titration and monochromatic ultraviolet spectrometry. Two commercial paste-type chelators containing ethylenediaminetetraacetic acid (EDTA) and peroxide (RC-Prep and Glyde) served as controls. Calcium-binding capacities were measured in mixtures with a Ca2+ standard solution buffered at pH 10 using a calcium-selective measuring chain. Finally, root canals of 16 extracted single-rooted premolars per group were instrumented using ProFile instruments dipped in the experimental gel, RC-Prep, or nothing. Additionally, canals were rinsed with 10 mL of a 1% NaOCl solution during/after preparation. Smear scores in instrumented teeth were monitored using scanning electron microscopy. None of the experimental gel components showed short-term interactions with hypochlorite, whilst EDTA, peroxide, RC-Prep and Glyde immediately reduced the hypochlorite in solution. The experimental gel chelated 30 mg Ca2+ g-1, compared with 16 mg Ca2+ g-1 and 11 mg Ca2+ g-1 chelated by RC-Prep and Glyde respectively. Smear scores obtained with the experimental gel were significantly (P<0.05) lower than with RC-Prep in coronal and middle root thirds, whilst no differences were observed in apical root thirds. Under the conditions of this study, an HEBP gel appeared advantageous over currently available products.

  6. Copper(II) complexes with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid: Syntheses, crystal structures and antifungal activities

    Energy Technology Data Exchange (ETDEWEB)

    Xiong, Pingping [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi' an 710069 (China); Li, Jie [Key Laboratory of Resource Biology and Biotechnology in Western China (Ministry of Education), Shaanxi Provincial Key Laboratory of Biotechnology, Xi' an 710069 (China); Bu, Huaiyu, E-mail: 7213792@qq.com [Key Laboratory of Resource Biology and Biotechnology in Western China (Ministry of Education), Shaanxi Provincial Key Laboratory of Biotechnology, Xi' an 710069 (China); Wei, Qing [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi' an 710069 (China); Zhang, Ruolin [Key Laboratory of Resource Biology and Biotechnology in Western China (Ministry of Education), Shaanxi Provincial Key Laboratory of Biotechnology, Xi' an 710069 (China); Chen, Sanping, E-mail: sanpingchen@126.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi' an 710069 (China)

    2014-07-01

    Reaction of Cu(II) with an asymmetric semi-rigid organic ligand 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid (HL), yielded five compounds, [Cu{sub 0.5}L]{sub n} (1), [Cu(HL){sub 2}Cl{sub 2}]{sub n} (2), [Cu(HL){sub 2}Cl{sub 2}(H{sub 2}O)] (3), [Cu(L){sub 2}(H{sub 2}O)]{sub n} (4) and [Cu(L)(phen)(HCO{sub 2})]{sub n} (5), which have been fully characterized by infrared spectroscopy, elemental analysis, and single-crystal X-ray diffraction. As for compounds 1, 2 and 5, Cu(II) is bridged through HL, Cl{sup -}, and formic acid, respectively, featuring 1D chain-structure. In compound 3, Cu(II) with hexahedral coordination sphere is assembled through hydrogen-bonding into 3D supramolecular framework. In compound 4, 1D chain units –Cu–O–Cu–O– are ligand-bridged into a 3D network. All compounds were tested on fungi (Fusarium graminearum, Altemaria solani, Macrophoma kawatsukai, Alternaria alternata and Colletotrichum gloeosporioides). Compound 1 exhibits a better antifungal effect compared to other compounds. An effect of structure on the antifungal activity has also been correlated. - Graphical abstract: Copper(II) compounds with 4-(1H-1, 2, 4-trizol-1-ylmethyl) benzoic acid, were prepared, structurally characterized and investigated for antifungal activity. - Highlights: • The title compounds formed by thermodynamics and thermokinetics. • The five compounds show higher inhibition percentage than reactants. • The structure effect on the antifungal activity.

  7. 2-[(3,5-Dimethyl-1-phenyl-1H-pyrazol-4-ylmethylene]indane-1,3-dione

    Directory of Open Access Journals (Sweden)

    Abdullah M. Asiri

    2011-02-01

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

  8. 2,4,6-Tri-amino-1,3,5-triazin-1-ium 3-(prop-2-eno-yloxy)propano-ate acrylic acid monosolvate monohydrate.

    Science.gov (United States)

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

    2013-05-01

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

  9. A coordination polymer of CdII with benzene-1,3-dicarboxylate and 1,4-bis[1-(2-pyridylmethylbenzimidazol-2-yl]butane

    Directory of Open Access Journals (Sweden)

    Wei-Ping Zhang

    2009-11-01

    Full Text Available The title CdII coordination polymer, catena-poly[[{1,4-bis[1-(2-pyridylmethylbenzimidazol-2-yl]butane}cadmium(II]-μ-benzene-1,3-dicarboxylato], [Cd(C8H4O4(C30H28N6]n, was obtained by reaction of CdCO3, benzene-1,3-dicarboxylic acid (H2btc and 1,4-bis[1-(2-pyridylmethylbenzimidazol-2-yl]butane (L. The CdII cation is six-coordinated by an N2O4-donor set. L acts as a bidentate ligand and btc anions link CdII centers into a chain propagating parallel to [010].

  10. 4-Aza-1-azoniabicyclo[2.2.2]octane–2-aminobenzoate–2-aminobenzoic acid (1/1/1

    Directory of Open Access Journals (Sweden)

    Hadi D. Arman

    2011-11-01

    Full Text Available A 4-aza-1-azoniabicyclo[2.2.2]octane cation, a 2-aminobenzoate anion and a neutral 2-aminobenzoic acid molecule comprise the asymmetric unit of the title compound, C6H13N2+·C7H6NO2−·C7H7NO2. An intramolecular N—H...O hydrogen bond occurs in the anion and in the neutral 2-aminobenzoic acid molecule. The cation provides a charge-assisted N—H...O hydrogen bond to the anion, and the 2-aminobenzoic acid molecule forms an O—H...N hydrogen bond to the unprotonated amino N atom in the cation. In this way, a three-component aggregate is formed. These are connected into a three-dimensional network by amino–carboxylate N—H...O hydrogen bonds. N—H...N hydrogen bonds are also observed.

  11. 2-([1,2,4]triazolo[1,5-c]quinazolin-2-yl-alkyl-(alkaryl-, aryl--amines and their derivatives. (3Н-quinazolin-4-ylidenhydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-ylalkyl-(alkaryl-, aryl-carboxylic acids: features of synthesis, modification and ant

    Directory of Open Access Journals (Sweden)

    Yu. V. Martynenko

    2016-08-01

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

  12. Synthesis of 1-(4-methylsulfone-phenyl)-5-(4-fluoro-phenyl)-5-[14C]-1,2,3- triazole and 1-(4-sulfonamide-phenyl)-5-(4-fluoro-phenyl)-5-[14C]-1,2,3- triazole as novel carbon-14 anticonvulsant

    International Nuclear Information System (INIS)

    Saemian, N.; Shirvani, G.; Matloubi, H.

    2006-01-01

    Two 1,2,3-triazole anticonvulsants, 1-(4-methylsulfone-phenyl)-5-(4-fluoro-phenyl)-5-[ 14 C]-1,2,3-triazole and 1-(4-sulfonamide-phenyl)-5-(4- fluoro-phenyl)-5-[ 14 C]-1,2,3-triazole, both labeled with carbon-14 in the 5-position were prepared from para-fluoro-benzonitrile-[cyano- 14 C]. (author)

  13. Tetraphenylphosphonium iodide–1,3,5-trifluoro-2,4,6-triiodobenzene–methanol (3/4/1

    Directory of Open Access Journals (Sweden)

    Gabriella Cavallo

    2013-06-01

    Full Text Available The crystallization of a 1:1 molar solution of 1,3,5-trifluoro-2,4,6-diiodobenzene (TFTIB and tetraphenylphosponium iodide (TPPI from methanol produced tetragonal needles of pure TPPI and tabular pseudo-hexagonal truncated bipyramids of the title compound, 3C24H20P+·3I−·4C6F3I3·CH4O or (TPPI3(TFTIB4·MeOH. The asymmetric unit is composed of six TPPI molecules, eight TFTIB molecules and two methanol molecules, overall 16 constituents. The formation of the architecture is essentially guided by a number of C—I...I− halogen bonds (XB, whose lengths are in the range 3.276 (1–3.625 (1 Å. Layers of supramolecular polyanions are formed parallel to (10-1 wherein iodide anions function as penta-, tetra- or bidentate XB acceptors. The structure is not far from being P21/n, but the centrosymmetry is lost due to a different conformation of a single couple of cations and the small asymmetry in the formed supramolecular anion. One methanol molecule is hydrogen bonded to an iodide anion, while the second is linked to the first one via an O—H...O contact. This second methanol molecule is more loosely pinned in its position than the first and presents very high anisotropic displacement parameters and a seeming shortening of the C—O bond length. The crystal studied was refined as a perfect inversion twin.

  14. Cloning, purification and crystallization of Thermus thermophilus proline dehydrogenase

    Energy Technology Data Exchange (ETDEWEB)

    White, Tommi A.; Tanner, John J., E-mail: tannerjj@missouri.edu [Departments of Chemistry and Biochemistry, University of Missouri-Columbia, Columbia, Missouri 65211 (United States)

    2005-08-01

    Cloning, purification and crystallization of T. thermophilus proline dehydrogenase is reported. The detergent n-octyl β-d-glucopyranoside was used to reduce polydispersity, which enabled crystallization. Nature recycles l-proline by converting it to l-glutamate. This four-electron oxidation process is catalyzed by the two enzymes: proline dehydrogenase (PRODH) and Δ{sup 1}-pyrroline-5-carboxylate dehydrogenase. This note reports the cloning, purification and crystallization of Thermus thermophilus PRODH, which is the prototype of a newly discovered superfamily of bacterial monofunctional PRODHs. The results presented here include production of a monodisperse protein solution through use of the detergent n-octyl β-d-glucopyranoside and the growth of native crystals that diffracted to 2.3 Å resolution at Advanced Light Source beamline 4.2.2. The space group is P2{sub 1}2{sub 1}2{sub 1}, with unit-cell parameters a = 82.2, b = 89.6, c = 94.3 Å. The asymmetric unit is predicted to contain two protein molecules and 46% solvent. Molecular-replacement trials using a fragment of the PRODH domain of the multifunctional Escherichia coli PutA protein as the search model (24% amino-acid sequence identity) did not produce a satisfactory solution. Therefore, the structure of T. thermophilus PRODH will be determined by multiwavelength anomalous dispersion phasing using a selenomethionyl derivative.

  15. Antimicrobial and antifungal activity of some (5-(adamantane-1-yl-4R-1,2,4-triazole-3-ylthiols substitutes

    Directory of Open Access Journals (Sweden)

    V. M. Odyntsova

    2016-12-01

    Full Text Available Lately adamantine containing substances have found wide use among the skeleton derivatives. The combination of adamantane and 1,2,4-triazole in one molecule creates significant preconditions to design new potential drugs with low toxicity and pronounced pharmacological activity. The aim of the research is the study of antimicrobial and antifungal activity of (5-(adamantane-1-yl-4-R-1,2,4-triazole-3-ylthiols substitutes. Materials and methods. Determination of antimicrobial and antifungal activity has been carried out by 2-fold serial dilutions method in liquid nutrient media. The substance of the antibacterial drug Trimethoprim has been applied as a control in determining antimicrobial activity of the compounds against the investigated strains of microorganisms. Results. According to the data of experiments the 5-(((5-(adamantane-1-yl-4-ethyl-4H-1,2,4-triazole-3-ylthiomethyl-4-ethyl-4H-1,2,4-triazole-3-thiol shows the same activity as Trimethoprim against P. aeruginosa (MIC is 62.5 µg/ml, MBC – 125 μg/ml, marked activity towards S. aureus (MIC is 15.6 μg/ml, MBC – 31.25 μg/ml while trimethoprim – 31.25 μg/ml, MBC – 62.5 µg/ml, greater fungistatic and fungicidal activity towards C. albicans, which amounted to 31.25 µg/ml, MFC – 62.5 µg/ml (while trimethoprim 62.5 µg/ml, MFC – 125 µg/ml. Reconstration of benzyldenhydrazide group to hydrazide one leads to the slight increase of bacteriostatic activity. Replacing the radical R from -Н to -C2H5 does not influence on the change of fungistatic activity. However, this resulted to the decrease in bacteriostatic activity against E. coli. The same is observed in relation to P. aeruginosa: from 62.5 μg/ml, MFC – 125 mcg/ml to 125 μg/ml, MFC – 125 µg/m respectively. Conclusion. The conducted study has showed that among the synthesized compounds there are some substances which strength of the antimicrobial and antifungal action in some cases exceeds the standard of comparison

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

    Science.gov (United States)

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

    2003-02-01

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

  17. Vapor-Liquid Equilibrium in the Mixture 1,1-Difluoroethane C2H4F2 + C4H8 2-Methylpropene (EVLM1131, LB5730_E)

    Science.gov (United States)

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

    This document is part of Subvolume A 'Binary Liquid Systems of Nonelectrolytes I' of Volume 26 'Heats of Mixing, Vapor-Liquid Equilibrium, and Volumetric Properties of Mixtures and Solutions' of Landolt-Börnstein Group IV 'Physical Chemistry'. It contains the Chapter 'Vapor-Liquid Equilibrium in the Mixture 1,1-Difluoroethane C2H4F2 + C4H8 2-Methylpropene (EVLM1131, LB5730_E)' providing data from direct measurement of pressure and mole fraction in vapor phase at variable mole fraction in liquid phase and constant temperature.

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  19. Ddc2 mediates Mec1 activation through a Ddc1- or Dpb11-independent mechanism.

    Directory of Open Access Journals (Sweden)

    Amitava Bandhu

    2014-02-01

    Full Text Available The protein kinase Mec1 (ATR ortholog and its partner Ddc2 (ATRIP ortholog play a key role in DNA damage checkpoint responses in budding yeast. Previous studies have established the model in which Ddc1, a subunit of the checkpoint clamp, and Dpb11, related to TopBP1, activate Mec1 directly and control DNA damage checkpoint responses at G1 and G2/M. In this study, we show that Ddc2 contributes to Mec1 activation through a Ddc1- or Dpb11-independent mechanism. The catalytic activity of Mec1 increases after DNA damage in a Ddc2-dependent manner. In contrast, Mec1 activation occurs even in the absence of Ddc1 and Dpb11 function at G2/M. Ddc2 recruits Mec1 to sites of DNA damage. To dissect the role of Ddc2 in Mec1 activation, we isolated and characterized a separation-of-function mutation in DDC2, called ddc2-S4. The ddc2-S4 mutation does not affect Mec1 recruitment but diminishes Mec1 activation. Mec1 phosphorylates histone H2A in response to DNA damage. The ddc2-S4 mutation decreases phosphorylation of histone H2A more significantly than the absence of Ddc1 and Dpb11 function does. Our results suggest that Ddc2 plays a critical role in Mec1 activation as well as Mec1 localization at sites of DNA damage.

  20. 1,1´,1´´-(2,4,6-Trihydroxybenzene-1,3,5-triyl)triethanone tautomerism revisited

    DEFF Research Database (Denmark)

    Hansen, Poul Erik; Kamounah, Fadhil S.; Zhiryakova, Diana

    2014-01-01

    It has recently been suggested that 1,1′,1′′-(2,4,6-trihydroxybenzene-1,3,5-triyl)triethanone may be tautomeric. Using 13C NMR chemical shifts and deuterium isotope effects on 13C chemical shifts, it is demonstrated that this is not the case. This compound occurs as a strongly hydrogen bonded ben...

  1. Extraction of Uranium in The Mixtures of Nitric and Sulfuric Acids With Neutral and Basic Ligands in Kerosene

    International Nuclear Information System (INIS)

    Nampira, Y; Rahayu Imam, S; Djoyosubroto, H

    1998-01-01

    The tendency of uranium ion in the mixture of nitric and sulfuric acid's medium is to from uranyl sulphate complex. The compound of uranyl sulphate is containing into the heteropoly compound that has acid property. Regarding to the mentioned property, the U extraction process was carried out using a basic or neutral complexing agent containing a ligand that formed the soluble uranium complex in the organic solvent (kerosene).The use of basic complexing agent such as n,tri-octyl amine is more suitable than that of tri butyl phosphate as a neutral agent. The maximum distribution coefficient of uranium will be reached if the maximum concentration of nitric acid and sulphuric acid can be maintained at 0.3 M and 1.5 M respectively in the organic solvent medium consisted n,tri-octyl amine of 30% volume fraction

  2. Study of hypercharge exchange processes 0{sup -}1/2+{yields}1{sup -} 1/2+; Estudio de procesos 0-1/2+{yields}1-1/2+ con intercambio de hipercarga

    Energy Technology Data Exchange (ETDEWEB)

    Albajar Molera, M c; Aguilar Beniter de Lugo, M.

    1981-07-01

    In this work we present a formalism for the reconstruction of the transitivity amplitudes governing the processes of the type 0-1/2+{yields}1-1/2+. The formalism uses the information contained in the decay angular correlations and takes into account the existence of mixed spin configurations in the final state 0-1/2+{yields}(0{down_arrow}, 1-)1/2+ (Author) 10 refs.

  3. Cocrystals of the antimalarial drug 11-azaartemisinin with three alkenoic acids of 1:1 or 2:1 stoichiometry.

    Science.gov (United States)

    Nisar, Madiha; Wong, Lawrence W Y; Sung, Herman H Y; Haynes, Richard K; Williams, Ian D

    2018-06-01

    The stoichiometry, X-ray structures and stability of four pharmaceutical cocrystals previously identified from liquid-assisted grinding (LAG) of 11-azaartemisinin (11-Aza; systematic name: 1,5,9-trimethyl-14,15,16-trioxa-11-azatetracyclo[10.3.1.0 4,13 .0 8,13 ]hexadecan-10-one) with trans-cinnamic (Cin), maleic (Mal) and fumaric (Fum) acids are herein reported. trans-Cinnamic acid, a mono acid, forms 1:1 cocrystal 11-Aza:Cin (1, C 15 H 23 NO 4 ·C 9 H 8 O 2 ). Maleic acid forms both 1:1 cocrystal 11-Aza:Mal (2, C 15 H 23 NO 4 ·C 4 H 4 O 4 ), in which one COOH group is involved in self-catenation, and 2:1 cocrystal 11-Aza 2 :Mal (3, 2C 15 H 23 NO 4 ·C 4 H 4 O 4 ). Its isomer, fumaric acid, only affords 2:1 cocrystal 11-Aza 2 :Fum (4). All cocrystal formation appears driven by acid-lactam R 2 2 (8) heterosynthons with short O-H...O=C hydrogen bonds [O...O = 2.56 (2) Å], augmented by weaker C=O...H-N contacts. Despite a better packing efficiency, cocrystal 3 is metastable with respect to 2, probably due to a higher conformational energy for the maleic acid molecule in its structure. In each case, the microcrystalline powders from LAG were useful in providing seeding for the single-crystal growth.

  4. Evaluation of the permeability of the furcation area of deciduous molars conditioned with Er:YAG laser and cyanoacrylate Avaliação da permeabilidade da região da furca de molares decíduos condicionada com laser de Er:YAG e cianoacrilatos

    Directory of Open Access Journals (Sweden)

    Adriene Mara Souza Lopes-Silva

    2003-09-01

    Full Text Available The purpose of this study was to evaluate in vitro the dentin permeability of the deciduous pulp chamber floor after employing 2-octyl cyanoacrylate and Er:YAG laser. Twenty four deciduous molars were used, divided into four groups. After chemical-surgical preparation each group received a different treatment: Group 1 - control, without treatment; Group 2 - the floor of the pulp chamber was covered with a fine layer of 2-octyl cyanoacrylate; Group 3 - the floor of the pulp chamber was irradiated with Er:YAG laser (250 mJ, 10 Hz for 30 seconds, 80 J of energy and 320 pulses, and covered with a fine layer of 2-octyl cyanoacrylate; and Group 4 - the floor of the pulp chamber was irradiated with Er:YAG laser set at the parameters already described. After that the specimens received application of 0.5% methylene blue, for 15 minutes. The teeth were cut, photographed, and the digitalized images were analyzed using the ImageLab program. The results obtained were submitted to statistical analysis. Group 4 (Er:YAG presented the largest averages in percentage of dye penetration area (19.5%, followed by Group 1 (11.1%, Group 3 (1.4% and Group 2 (0.2%. The experimental model allowed to conclude that the specimens conditioned with 2-octyl cyanoacrylate (Group 2 and Er:YAG laser associated to 2-octyl cyanoacrylate (Group 3 presented a decrease in permeability, and the specimens treated with Er:YAG laser (Group 4 presented an increase in permeability of the analyzed area.A proposta do presente experimento foi avaliar in vitro a permeabilidade da dentina no assoalho da câmara pulpar de dentes decíduos com o emprego do 2-octil cianoacrilato e laser de Er:YAG. Foram empregados 24 molares decíduos, divididos em quatro grupos. Após preparo químico-cirúrgico, cada grupo recebeu um tratamento diferente: Grupo 1 - controle, sem tratamento; Grupo 2 - o assoalho da câmara pulpar foi coberto com uma fina camada de 2-octil cianoacrilato; Grupo 3 - o assoalho da c

  5. Synthesis and structure of new 4-amino-5-(2-R1-phenyl-1,2,4-triazole-3-thiol alkilderivatives

    Directory of Open Access Journals (Sweden)

    Ye. S. Pruglo

    2017-08-01

    Full Text Available Chemistry of heterocyclic systems is a separate branch of organic chemistry with a long history and future prospects. The ring system of 1,2,4-triazole continuously attracts the interest of chemists, pharmacologists and pharmacists in finding medicinal compounds through its universal potential interactions with biological systems. Today it is known that 1,2,4-triazole derivatives have antibacterial, antifungal, antiinflammatory, anticonvulsant, antiviral, antituberculosis, antioxidant, anticancer and antitumor activities. They also have analgesic, local anesthetic, antimalarial, antiproliferative effects, antihypertensive, antidepressant, sedative, antihistamine, hepatoprotective, hypoglycemic, diuretic, antipyretic and countless number of action types. Therefore, the search of biologically active remedies and creating of new drugs on its base is highly efficient topical issue of medical and pharmaceutical work. The purpose of these studies is the synthesis, establishment of physical-chemical parameters of new 4-amino-5-(2-R1-phenyl-1,2,4-triazole-3-thiol alkylderivatives. Materials and methods. The studying of physical and chemical properties of compounds was made in accordance with the methods described in the State Pharmacopoeia of Ukraine 2.0. The melting point was determined on an automatic gear MPA100. The elemental composition of the compounds was set on the analyzer Elementar Vario EL cube. 1H NMR spectra were recorded using the spectrometer Varian Mercury VX-200 (1H, 200 MHz and decrypted by a computer program SpinWorks 3.1.8. Chromatography-mass spectral studies were carried out in the gas-liquid chromatograph Agilent 1260 Infinity HPLC equipped with a mass spectrometer Agilent 6120 (in electrospray ionization (ESI. Results. 4-amino-5-phenyl-4H-1,2,4-triazole-3-thiol and 4-amino-5-(2-bromophenyl-4H-1,2,4-triazol-3-thiol were used as the initial materials. These compounds were obtained by reaction of benzoic acid hydrazide and 2

  6. {4-Phenyl-1-[1-(1,3-thiazol-2-ylethylidene]thiosemicarbazidato}{4-phenyl-1-[1-(1,3-thiazol-2-ylethylidene]thiosemicarbazide}nickel(II chloride monohydrate

    Directory of Open Access Journals (Sweden)

    Ramaiyer Venkatraman

    2010-05-01

    Full Text Available In the title compound, [Ni(C12H11N4S2(C12H12N4S2]Cl·H2O, the NiII ion is chelated by two 2-acetylthiazole-3-phenylthiosemicarbazone ligands, forming a distorted octahedral complex. The metal ion is coordinated via the thiazole nitrogen, imine nitrogen and thione sulfur atoms from each thiosemicarbazone ligand, and two coordinating units lie almost perpendicular to each other give dihedral angle = 81.89 (1°]. One thiosemicarbazone unit is found to bind a chloride anion through two hydrogen bonds, while the other is linked with the disordered crystal water molecule. Two molecules are connected to each other through an intermolecular N—H...S interaction, forming a centrosymmetric dimer. Dimers are linked into sheets by π–π stacking of two phenyl rings [shortest C...C distance = 4.041 (3 Å].

  7. Chemistry of CCl 4 on Fe 3O 4(1 1 1)-(2 × 2) surfaces in the presence of adsorbed D 2O studied by temperature programmed desorption

    Science.gov (United States)

    Adib, K.; Totir, G. G.; Fitts, J. P.; Rim, K. T.; Mueller, T.; Flynn, G. W.; Joyce, S. A.; Osgood, R. M.

    2003-07-01

    Temperature programmed desorption (TPD) was used to study surface reactions of Fe 3O 4(1 1 1)-(2 × 2) sequentially exposed, at ˜100 K, to vapor-phase D 2O and CCl 4. Previous TPD and XPS results have indicated that in the absence of D 2O, CCl 4 dissociatively adsorbs on Fe 3O 4(1 1 1) producing chemisorbed Cl and CCl 2. Subsequent heating of the surface results in abstraction of lattice iron and oxygen atoms and causes them to desorb as FeCl 2 and OCCl 2, respectively. This study shows that when this Fe 3O 4 surface is exposed only to D 2O, TPD measures a rich surface chemistry with multiple desorption events extending as high as ˜800 K, indicating dissociative adsorption of D 2O on the Fe 3O 4(1 1 1) surface. After sequential exposure to D 2O and then CCl 4, the production of FeCl 2 and OCCl 2 from adsorbed CCl 4 is suppressed, indicating that D 2O fragments block the surface reactive sites.

  8. Emissions in potassium vapour under 4S1/2-7S1/2 two-photon nsec excitation

    International Nuclear Information System (INIS)

    Pentaris, D.; Chatzikyriakos, G.; Armyras, A.; Efthimiopoulos, T.

    2010-01-01

    The two-photon excitation of 4S 1/2 -7S 1/2 transition of potassium atoms is studied. Several coherent emissions and processes are possible, such as parametric four-wave (PFWM), parametric six-wave (PSWM) mixing and competition with the stimulated hyper Raman (SHRS) and the amplified spontaneous emission (ASE). The radiations at the transitions 6P 3/2,1/2 -4S 1/2 , 6S 1/2 -4P 3/2,1/2 and 5P 3/2,1/2 -4S 1/2 are emitted only in the forward direction (indicating a parametric process), while the radiation at the transition 4P 3/2,1/2 -4S 1/2 is emitted in the forward and in the backward direction, indicating an ASE process.

  9. The crystal structure of 6-(4-chlorophenyl-2-(4-methylbenzylimidazo[2,1-b][1,3,4]thiadiazole-5-carbaldehyde

    Directory of Open Access Journals (Sweden)

    A. Sowmya

    2016-10-01

    Full Text Available In the title imidazo[2,1-b][1,3,4]thiadiazole derivative, C19H14ClN3OS, the 4-methylbenzyl and chlorophenyl rings are inclined to the planar imidazo[2,1-b][1,3,4]thiadiazole moiety (r.m.s. deviation = 0.012 Å by 64.5 (1 and 3.7 (1°, respectively. The molecular structure is primarily stabilized by a strong intramolecular C—H...O hydrogen bond, leading to the formation of a pseudo-seven-membered S(7 ring motif, and a short intramolecular C—H...N contact forming an S(5 ring motif. In the crystal, molecules are linked by pairs of C—H...S hydrogen bonds, forming inversion dimers. The dimers are linked by C—H...O and C—H...π interactions, forming chains propagating along [110].

  10. Single-electron transfer in palladium complexes of 1,4-naphthoquinone-containing bis(pyrazol-1-yl)methane ligands.

    Science.gov (United States)

    Scheuermann, Sebastian; Sarkar, Biprajit; Bolte, Michael; Bats, Jan W; Lerner, Hans-Wolfram; Wagner, Matthias

    2009-10-05

    A 1,4-naphthoquinone-substituted bis(pyrazol-1-yl)methane ligand (N--N) has been synthesized and transformed into its corresponding Pd(II) chelate complex [(N--N)PdCl(2)]. Both N--N and [(N--N)PdCl(2)] have been fully characterized by NMR spectroscopy, spectro-electrochemistry, and X-ray crystallography. After treatment of [(N--N)PdCl(2)] with NEt(3), the signature of a 1,4-naphthosemiquinonate radical is visible in the UV-vis- and electron paramagnetic resonance (EPR) spectrum of the reaction mixture; the free ligand N--N does not react with NEt(3) under the conditions applied. It is therefore concluded that NEt(3) first reduces the Pd(II)-ion of [(N--N)PdCl(2)] to the zero-valent state and that this reaction is followed by a single-electron transfer from the metal atom to the 1,4-naphthoquinone moiety. The complex has been specifically designed to disfavor any direct Pd-to-naphthoquinone coordination. Electron transfer thus proceeds through space or, less likely, via sigma-bonds of the ligand framework.

  11. Synthesis and Antibacterial Activity of 1,3,4-Oxadiazole and 1,2,4 ...

    African Journals Online (AJOL)

    NJD

    The antibacterial activities of the starting materials, the synthetic intermediates and the products were tested and are reported below. 2. Results and Discussion. 2.1. Synthesis. The final products 4, 6, 8 and 9 have been synthesized by a common pathway as summarized in Scheme 1. The methyl salicylate 2 was synthesized ...

  12. In Vitro Antioxidant Evaluation of Some Mannich Bases which Contain Bis-1,2,4 -Triazole Derivative

    International Nuclear Information System (INIS)

    Parlak, A. E.; Karatepe, M.; Koparir, M.; Alayunt, N. O.; Keser, S.; Dastan, S. D.; Ulas, M.; Celik, S.

    2015-01-01

    This study aims to examine the antioxidant effects of some Mannich bases containing bis-1, 2, 4 triazole, which are synthesized afresh. The antioxidant activities of the derivatives were measured using different methods in this study, including reducing power capacity, metal chelating activity, superoxide anion radicals scavenging activity, H/sub 2/ O/sub 2/ scavenging activity and hydroxyl radical scavenging. As a result, derivatives had efficient antioxidant and free radical scavenging activity when compared to ascorbic acid, BHT and alpha-tocopherol as associated antioxidants. (author)

  13. Synthesis and Preliminary Cytotoxicity Studies of 1-[1-(4,5-Dihydrooxazol- 2-yl)-1H-indazol-3-yl]-3-phenylurea and 3-phenylthiourea Derivatives.

    Science.gov (United States)

    Kornicka, Anita; Saczewski, Franciszek; Bednarski, Patrick J; Korcz, Martyna; Szumlas, Piotr; Romejko, Ewa; Sakowicz, Aneta; Sitek, Lukasz; Wojciechowska, Monika

    2017-01-01

    N-substituted 3-amino-1H-indazoles represent an interesting class of biologically active compounds. Among them, derivatives containing phenylurea moiety are of particular interest. Such compounds have been found to possess inhibitory activity against cancer cell growth. Additionally, various oxazoline-containing compounds have also been designed as potential anticancer agents. The aim of this work was to obtain a new class of N-substituted 3-amino-1H-indazole derivatives with cytotoxic activity towards cancer cells. Two series of 1-[1-(4,5-dihydrooxazol-2-yl)-1H-indazol-3-yl]-3-phenylurea and 3- phenylthiourea derivatives 7-17 and 18-22, respectively, were prepared and screened for their potential in vitro cytotoxic activities against lung carcinoma LCLC-103H cell line using a crystal violet microtiter plate assay. All the urea derivatives, except the compound 8, were inactive at a concentration of 20 μM attainable in cancer cells, while the thiourea derivatives showed a pronounced cancer cell growth inhibitory effects. The most potent 1-[1-(4,5-dihydrooxazol-2-yl)-1H-indazol-3-yl]-3-ptolylthiourea (19) exhibited cytotoxicity on the lung cancer LCLC-103H and cervical cancer SISO cell lines at a concentration of 10 µM. Moreover, compound 19 displayed cytostatic activity against pancreas cancer DAN-G cell line. The 1-[1-(4,5-dihydrooxazol-2-yl)-1H-indazol-3-yl]-3-phenylthiourea derivatives described herein may serve as a useful scaffold for the search for novel anticancer agents. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  14. Crystal structure of 4,4′-bis[3-(piperidin-1-ylprop-1-yn-1-yl]-1,1′-biphenyl

    Directory of Open Access Journals (Sweden)

    Anqi Walbaum

    2017-06-01

    Full Text Available The title compound, C28H32N2, (I, is one of a second generation of compounds designed and synthesized based on a very potent and selective α9α10 nicotinic acetylcholine receptor antagonist ZZ161C {1,1′-[[1,1′-biphenyl]-4,4′-diylbis(prop-2-yne-3,1-diyl]bis(3,4-dimethylpyridin-1-ium bromide}, which has shown analgesic effects in a chemotherapy-induced neuropathy animal model. Compound (I was synthesized by the reaction of 4,4′-bis(3-bromoprop-1-yn-1-yl-1,1′-biphenyl with piperidine at room temperature in acetonitrile. The single-crystal used for X-ray analysis was obtained by dissolving (I in a mixture of dichloromethane and methanol, followed by slow evaporation of the solvent. In the crystal of (I, the biphenyl moiety has a twisted conformation, with a dihedral angle of 25.93 (4° between the benzene rings. Both piperidine head groups in (I are in the chair conformation and are oriented so that the N-atom lone pairs of each piperidine group point away from the central biphenyl moiety.

  15. 1,3-Diphenyl-3,4-dihydrobenzo[b][1,6]naphthyridine

    Directory of Open Access Journals (Sweden)

    Werner Seebacher

    2010-05-01

    Full Text Available The title compound, C24H18N2, is the first structural example containing the 3,4-dihydrobenzo[b][1,6]naphthyridine fragment. It was synthesized from 2,4,6,8-tetraphenyl-3,7-diazabicyclo[3.3.1]nonan-9-one and was crystallized from a methanol–ethanol solution over two years as a racemate. The C=N double bond [1.2868 (15 Å] is bent significantly out of the plane of the aromatic bicyclic ring system [N—C—C—C = −157.63 (12°] and out of the plane of the phenyl ring bonded at the 1-position [N—C—C—C = 41.15 (16°].

  16. Study of hypercharge exchange processes 0-1/2+→1- 1/2+

    International Nuclear Information System (INIS)

    Albajar Molera, M. c.; Aguilar Beniter de Lugo, M.

    1981-01-01

    In this work we present a formalism for the reconstruction of the transitivity amplitudes governing the processes of the type 0-1/2+→1-1/2+. The formalism uses the information contained in the decay angular correlations and takes into account the existence of mixed spin configurations in the final state 0-1/2+→(0↓, 1-)1/2+ (Author) 10 refs

  17. 2-(1,3-Dioxoisoindolin-2-ylacetic acid–N′-[(E-2-methoxybenzylidene]pyridine-4-carbohydrazide (1/1

    Directory of Open Access Journals (Sweden)

    Shaaban K. Mohamed

    2012-08-01

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

  18. Studies on dechlorination of DDT (1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane) using magnesium/palladium bimetallic system

    International Nuclear Information System (INIS)

    Gautam, Sumit Kumar; Suresh, Sumathi

    2007-01-01

    The aim of our investigation was to compare the rates of dechlorination of DDT using Mg 0 /Pd 4+ system in two different reaction phases, namely, water-acetone and 0.05% biosurfactant in water. Since palladium is expensive and its toxicity effects are not well known we also examined the reuse efficiency of Pd 0 immobilized on alumina for dechlorinating DDT. Studies on the dechlorination of DDT in water-acetone (1:1, v/v) and 0.05% biosurfactant phases revealed that the reaction followed second order kinetics and rate of reaction is dependent upon both initial concentrations of the target compound and Mg 0 /Pd 4+ . The presence of acid enhanced the rate of reaction by providing protons and preventing passivation of metal that occurs due to deposition of magnesium hydroxide. GC-MS analyses revealed the formation of completely dechlorinated hydrocarbon skeleton of DDT namely, diphenylethane (DPE), as the end product in both reaction phases (water-acetone and 0.05% biosurfactant in water) thereby implying the removal of all five chlorine atoms (three alkyl and two aryl) of DDT. The optimum ratio of water and acetone to facilitate successful dechlorination reaction was found to be 9:1. Results suggested that salt form (K 2 PdCl 6 ) of palladium had higher potential to dechlorinate DDT as compared to pellet (Pd 0 -alumina) form (efficiencies of 95 and 36%, respectively, for 100 ppm initial concentration of DDT). We noted that Pd 0 -alumina pellets could be reused at least four times for successful dechlorination of DDT provided Mg 0 granules are present in sufficient quantity. Technical grade DDT (50 ppm) containing significant amounts of DDD was dechlorinated almost completely by the Mg 0 /Pd 4+ (10 mg/0.2 mg/ml) within 1 h in water-biosurfactant phase. Our studies reveal that Mg/Pd system is a promising option due to its high reactivity and its ability to achieve complete dechlorination of DDT. This bimetallic system may be useful for designing indigenous permeable

  19. Stereoselective reactions. XXXII. Enantioselective deprotonation of 4-tert-butylcyclohexanone by fluorine-containing chiral lithium amides derived from 1-phenylethylamine and 1-(1-naphthyl)ethylamine.

    Science.gov (United States)

    Aoki, K; Koga, K

    2000-04-01

    Enantioselective deprotonation of 4-tert-butylcyclohexanone was examined using 1-phenylethylamine- and 1-(1-naphthyl)ethylamine-derived chiral lithium amides having an alkyl or a fluoroalkyl substituent at the amide nitrogen. The lithium amides having a 2,2,2-trifluoroethyl group on the amide nitrogen are easily accessible in both enantiomeric forms, and were found to induce good enantioselectivity in the present reaction.

  20. Dihydroxylation of 4-substituted 1,2-dioxines

    DEFF Research Database (Denmark)

    Robinson, Tony V; Pedersen, Daniel Sejer; Taylor, Dennis K

    2009-01-01

    The synthesis of 2-C-branched erythritol derivatives, including the plant sugar (+/-)-2-C-methylerythritol 2, was achieved through a dihydroxylation/reduction sequence on a series of 4-substituted 1,2-dioxines 3. The asymmetric dihydroxylation of 1,2-dioxines was examined, providing access...... to optically enriched dihydroxy 1,2-dioxanes 4. The synthesized 1,2-dioxanes were converted to other erythro sugar analogues and tetrahydrofurans through controlled cleavage of the endoperoxide linkage....

  1. Solid solutions on the base of CuCr2Se4 and CUsUb(1/2)Insub(1/2)Crsub(2)Sesub(4)

    International Nuclear Information System (INIS)

    Smirnov, S.G.; Rozantsev, A.V.; Kesler, Ya.A.; Gordeev, I.V.; Tret'yakov, Yu.D.

    1983-01-01

    The CuCr 2 Se 4 interaction with Cusub(1/2)Insub(1/2)Crsub(2)Sesub(4) for determining the fields of solid solutions existence and studying their crystallochemical properties is investigated. Solid solutions of the (1-x)Cusub(1/2)Insub(1/2)Crsub(2)Sesub(4)xxCuCrsub(2)Sesub(4) are prepared, two limited regions of solid solutions of spinel type at 0 <= x <= 0.2 and 0.8 <= x <= 1 are determined. X-ray radiography investigation of synthesized solid solutions is carried out. It has been found that at 0 <= x <= 0.2 solid solutions are crystallized in the ordered spinel structure F anti 43m

  2. One-pot synthesis of novel 1-(1H-tetrazol-5-yl)-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine derivatives via an Ugi-azide 4CR process.

    Science.gov (United States)

    Ghandi, Mehdi; Salahi, Saleh; Taheri, Abuzar; Abbasi, Alireza

    2018-05-01

    A facile one-pot method has been developed for the synthesis of novel pyrrolo[2,1-a]pyrazine scaffolds. A variety of 1-(1H-tetrazol-5-yl)-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine derivatives were obtained in moderate to high yields in methanol using a one-pot four-component condensation of 1-(2-bromoethyl)-1H-pyrrole-2-carbaldehyde, amine, isocyanide and sodium azide at room temperature. These reactions presumably proceed via a domino imine formation, intramolecular annulation and Ugi-azide reaction. Unambiguous assignment of the molecular structures was carried out by single-crystal X-ray diffraction.

  3. 4-Aza-1-azoniabicyclo?[2.2.2]octa?ne?2-amino?benzoate?2-amino?benzoic acid (1/1/1)

    OpenAIRE

    Arman, Hadi D.; Kaulgud, Trupta; Tiekink, Edward R. T.

    2011-01-01

    A 4-aza-1-azoniabicyclo[2.2.2]octane cation, a 2-aminobenzoate anion and a neutral 2-aminobenzoic acid molecule comprise the asymmetric unit of the title compound, C6H13N2+·C7H6NO2−·C7H7NO2. An intramolecular N—H...O hydrogen bond occurs in the anion and in the neutral 2-aminobenzoic acid molecule. The cation provides a charge-assisted N—H...O hydrogen bond to the anion, and the 2-aminobenzoic acid molecule forms an O—H...N hydrogen bo...

  4. One-pot synthesis of 4,8-dibromobenzo[1,2-c;4,5-c']bis[1,2,5]thiadiazole.

    Science.gov (United States)

    Tam, Teck Lip; Li, Hairong; Wei, Fengxia; Tan, Ke Jie; Kloc, Christian; Lam, Yeng Ming; Mhaisalkar, Subodh G; Grimsdale, Andrew C

    2010-08-06

    A one-step synthesis of 4,8-dibromobenzo[1,2-c;4,5-c']bis[1,2,5]thiadiazole with use of 1,2,4,5-tetraaminobenzene tetrahydrobromide and thionyl bromide in good yield is reported. This unit can then be used in the synthesis of low bandgap materials via palladium-catalyzed coupling reactions. The approach offers a quick and easy way to prepare low bandgap materials as compared to the current literature methods.

  5. Efficient white organic light-emitting devices using a thin 4,4'-bis(2,2'-diphenylvinyl)-1,1'-diphenyl layer

    International Nuclear Information System (INIS)

    Wang Jun; Yu Junsheng; Li Lu; Tang Xiaoqing; Jiang Yadong

    2008-01-01

    White organic light-emitting devices (OLEDs) were fabricated using phosphorescent material bis[2-(4-tert-butylphenyl)benzothiazolato-N,C 2' ]iridium (acetylacetonate) [(t-bt) 2 Ir(acac)] doped in 4,4'-bis(carbazol-9-yl) biphenyl (CBP) matrix as a yellow light-emitting layer and a thin layer 4,4'-bis(2,2'-diphenylvinyl)-1,1'-diphenyl (DPVBi) as the blue light-emitting layer. The light colour of the OLEDs can be adjusted by changing doped concentration and the thickness of the DPVBi thin layer. The maximum luminance and power efficiency of 5% doped device reached 15 460 cd m -2 and 8.1 lm W -1 , respectively. The 3% doped device showed the CIE coordinates of (0.344, 0.322) at 8 V and a maximum power efficiency of 5.7 lm W -1 at 4.5 V

  6. (2,4-Dioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylato-κ2O4,O5(4-oxido-2-oxo-1,2-dihydropyrimidine-5-carboxylato-κ2O4,O5bis(1,10-phenanthroline-κ2N,N′yttrium(III dihydrate

    Directory of Open Access Journals (Sweden)

    Zilu Chen

    2008-09-01

    Full Text Available In the title compound, [Y(C5H2N2O4(C5H3N2O4(C12H8N22]·2H2O, the YIII ion lies on a twofold rotation axis and exhibits a distorted square-antiprismatic coordination geometry. It is chelated by two 1,10-phenanthroline ligands, a 2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate monoanion and a 4-oxido-2-oxo-1,2-dihydropyrimidine-5-carboxylate dianion. The H atom involved in an N—H...N hydrogen bond between the 1,2-dihydropyrimidine units has half occupancy and is disordered around a twofold rotation axis.

  7. Fragrance material review on 1-(3,3-dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one.

    Science.gov (United States)

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

    2013-12-01

    A toxicologic and dermatologic review of 1-(3,3-dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one when used as a fragrance ingredient is presented. 1-(3,3-Dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all available toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 1-(3,3-dimethylbicyclo[2.2.1]hept-2-yl)ethane-1-one were evaluated then summarized and includes physical properties, skin irritation, mucous membrane (eye) irritation, and skin sensitization data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (Belsito, D., Bickers, D., Bruze, M., Calow, P., Dagli, M., Fryer, A.D., Greim, H., Miyachi, Y., Saurat, J.H., Sipes, I.G., 2013. A Toxicologic and Dermatologic Assessment of Alkyl Cyclic Ketones When Used as Fragrance Ingredients (submitted for publication) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. An electrochemical study of the systems Li1+-xV2O4 and Li1-xVO2 (0≤x≤1)

    International Nuclear Information System (INIS)

    De Picciotto, L.A.; Thackeray, M.M.; Pistoia, G.

    1988-01-01

    Electrochemical properties of the systems Li 1±x V 2 O 4 (0≤x≤1), Li 1-x VO 2 (0≤x 2 O 4 is reversible, which confirms that lithium may be cycled, topotactically, in and out of the Li 1+x V 2 O 4 spinel structure. Delithiation of the LiV 2 O 4 spinel is irreversible; during this process the vanadium ions migrate through the oxide layers. This results in a defect rocksalt phase, which can, in turn, be relithiated by a different mechanism. Lithium extraction for the layered compound LiVO 2 yields a structure similar to the delithiated LiV 2 O 4 product. The spinel-derived compounds Li 1 +-x/V 2 O 4 (0 -3 Ω -1 cm -1 at x=0 and 10 -6 Ω -1 cm -1 at x=1. Lithium diffusion rates in Li 1±x V 2 O 4 samples increase with lithiation from D=4x10 -10 cm 2 /s in LiV 2 O 4 to D=6x10 -8 cm 2 /s in Li 2 V 2 O 4 . Intermediate values of D are obtained in the delithiated compound Li 0.28 V 2 O 4 and in the layered oxide LiVO 2 ; significantly lower values of D, viz. 1x10 -11 cm 2 /s and 4x10 -11 cm 2 /s , are found in the spinels LiMn 2 O 4 and Fe 3 O 4 respectively. 28 refs.; 5 figs.; 1 table

  9. SYNTHESIS, CHARACTERIZATION AND ANTIOXIDANT ACTIVITIES OF NOVEL 1-(MORPHOLINE-4-YL-METHYL-3-ALKYL(ARYL-4-[4-(DIMETHYLAMINO-BENZYLIDENAMINO]-4,5-DIHYDRO-1H-1,2,4-TRIAZOL-5-ONES

    Directory of Open Access Journals (Sweden)

    Özlem Gürsoy Kol

    2016-08-01

    Full Text Available In this paper, eight novel 1-(morpholine-4-yl-methyl-3-alkyl(aryl-4-[4-(dimethylamino-benzylidenamino]-4,5-dihydro-1H-1,2,4-triazol-5-ones (2 were obtained by the reactions of 3-alkyl(aryl-4-[4-(dimethylamino-benzylidenamino]-4,5-dihydro-1H-1,2,4-triazol-5-ones (1 with formaldehyde and morpholine. The novel synthesized compounds were identified by IR, 1H NMR and 13C NMR spectral data. Besides, the newly synthesized compounds were analysed for their in vitro potential antioxidant capacities in three different assays. All of the compounds demonstrated significant activity for metal chelating effect.

  10. Standard technical specifications: General Electric plants, BWR/4. Volume 1, Revision 1: Specifications

    International Nuclear Information System (INIS)

    1995-04-01

    This report documents the results of the combined effort of the NRC and the industry to produce improved Standard Technical Specifications (STS), Revision 1 for General Electric BWR/4 Plants. The changes reflected in Revision 1 resulted from the experience gained from license amendment applications to convert to these improved STS or to adopt partial improvements to existing technical specifications. This NUREG is the result of extensive public technical meetings and discussions between the Nuclear Regulatory Commission (NRC) staff and various nuclear power plant licensees, Nuclear Steam Supply System (NSSS) Owners Groups, NSSS vendors, and the Nuclear Energy Institute (NEI). The improved STS were developed based on the criteria in the Final Commission Policy Statement on Technical Specifications Improvements for Nuclear Power Reactors, dated July 22, 1993. The improved STS will be used as the basis for individual nuclear power plant licensees to develop improved plant-specific technical specifications. This report contains three volumes. Volume 1 contains the Specifications for all chapters and sections of the improved STS. Volume 2 contains the Bases for Chapters 2.0 and 3.0, and Sections 3.1--3.3 of the improved STS. Volume 3 contains the Bases for Sections 3.4--3.10 of the improved STS

  11. (S-2-(4-Chlorobenzoyl-1,2,3,4-tetrahydrobenzo[e]pyrazino[1,2-a][1,4]diazepine-6,12(11H,12aH-dione—Synthesis and Crystallographic Studies

    Directory of Open Access Journals (Sweden)

    Adam Mieczkowski

    2017-10-01

    Full Text Available (S-2-(4-Chlorobenzoyl-1,2,3,4-tetrahydrobenzo[e]pyrazino[1,2-a][1,4]diazepine-6,12(11H,12aH-dione was obtained in a three-step, one-pot synthesis, starting from optically pure (S-2-piperazine carboxylic acid dihydrochloride. Selective acylation of the β-nitrogen atom followed by condensation with isatoic anhydride and cyclization with HATU/DIPEA to a seven-member benzodiazepine ring, led to the tricyclic benzodiazepine derivative. Crystallographic studies and initial biological screening were performed for the title compound.

  12. Phenazine–naphthalene-1,5-diamine–water (1/1/2

    Directory of Open Access Journals (Sweden)

    Maria Gdaniec

    2009-12-01

    Full Text Available The asymmetric unit of the title compound, C12H8N2·C10H10N2·2H2O, contains one half-molecule of phenazine, one half-molecule of naphthalene-1,5-diamine and one water molecule. The phenazine and naphthalene-1,5-diamine molecules are located on inversion centers. The water molecules serve as bridges between the naphthalene-1,5-diamine molecules and also between the naphthalene-1,5-diamine and phenazine molecules. The naphthalene-1,5-diamine and water molecules are connected via N—H...O and O—H...N hydrogen bonds, forming a T4(2 motif. They are arranged into a two-dimensional polymeric structure parallel to (10overline{1} in which the water molecule is a single donor and a double acceptor, whereas the amino group is a double donor and a single acceptor in the hydrogen bonding. These two-dimensional assemblies alternate with the layers of phenazine molecules arranged into a herringbone motif. Each phenazine molecule is hydrogen bonded to two water molecules and thus a three-dimensional framework of hydrogen-bonded molecules is generated.

  13. Synthesis and solubility measurement in supercritical carbon dioxide of two solid derivatives of 2-methylnaphthalene-1,4-dione (menadione): 2-(Benzylamino)-3-methylnaphthalene-1,4-dione and 3-(phenethylamino)-2-methylnaphthalene-1,4-dione

    International Nuclear Information System (INIS)

    Zacconi, Flavia C.; Nuñez, Olga N.; Cabrera, Adolfo L.; Valenzuela, Loreto M.

    2016-01-01

    Highlights: • Two menadione derivatives were synthesized, purified and characterized. • Solubility of menadione derivatives in SC-CO 2 was measured at T < 333 K, p < 28 MPa. • Thermodynamic consistency of solubility data measured was evaluated. • Solubility data was correlated in terms of temperature and CO 2 density. - Abstract: Synthesis of two solid derivatives of vitamin K 3 (2-methylnaphthalene-1,4-dione or menadione), 2-(benzylamino)-3-methylnaphthalene-1,4-dione and 3-(phenethylamino)-2-methylnaphthalene-1,4-dione was completed using a 1,4 Michael addition reaction at 323 K in an inert atmosphere, with reaction yields of 62% mol·mol −1 and 71% mol·mol −1 , respectively, and a purity grade of 98% mol·mol −1 for each component. Isothermal solubility (mole fraction) of each solid derivative in supercritical carbon dioxide was performed using an analytic-recirculation methodology, with direct determination of the molar composition of the carbon dioxide-rich phase by using high performance liquid chromatography, at temperatures of (313, 323 and 333) K and pressures from (8–28) MPa. Results indicated that the range of measured solubilities were from (59 × 10 −6 to 368 × 10 −6 ) mol·mol −1 for solid 2-(benzylamino)-3-methylnaphthalene-1,4-dione and from (40 × 10 −6 to 205 × 10 −6 ) mol·mol −1 for solid 3-(phenethylamino)-2-methylnaphthalene-1,4-dione. The experimental solubility was validated using three approaches, estimating the combined expanded uncertainty of measurement for each solubility data point, evaluating the thermodynamic consistency of the data utilizing a test based on the Gibbs–Duhem equation, and verifying the self-consistency by correlating the experimental solubility values with a semi-empirical model as a function of temperature, pressure and pure carbon dioxide density.

  14. Gas chromatography-mass spectrometry analysis of di-n-octyl disulfide in a straight oil metalworking fluid: application of differential permeation and Box-Cox transformation.

    Science.gov (United States)

    Xu, Wenhai; Que Hee, Shane S

    2006-01-06

    The aim of this study was to identify and quantify an unknown peak in the chromatogram of a very complex mixture, a straight oil metalworking fluid (MWF). The fraction that permeated through a thin nitrile polymer membrane had less mineral oil background than the original MWF did at the retention time of the unknown peak, thus facilitating identification by total ion current (TIC) gas chromatography-mass spectrometry (GC-MS). The peak proved to be di-n-octyl disulfide (DOD) through retention time and mass spectral comparisons. Quantitation of DOD was by extracted ion chromatogram analysis of the DOD molecular ion (mass-to-charge ratio (m/z) 290), and of the m/z 71 ion for the internal standard, n-triacontane. Linear models of the area ratio (y) of these two ions versus DOD concentration showed a systematic negative bias at low concentrations, a common occurrence in analysis. The linear model of y(0.8) (from Box-Cox power transformation) versus DOD concentration showed negligible bias from the lowest measured standard of 1.51 mg/L to the highest concentration tested at 75.5 mg/L. The intercept did not differ statistically from zero. The concentration of DOD in the MWF was then calculated to be 0.398+/-0.034% (w/w) by the internal standard method, and 0.387+/-0.036% (w/w) by the method of standard additions. These two results were not significantly different at p Box-Cox transformation is therefore recommended when the data for standards are non-linear.

  15. Prodrug-activating Gene Therapy with Rabbit Cytochrome P450 4B1/4-Ipomeanol or 2-Aminoanthracene System in Glioma Cells

    Energy Technology Data Exchange (ETDEWEB)

    Jang, Su Jin; Kang, Joo Hyun; Lee, Tae Sup; Kim, Sung Joo; Kim, Kwang Il; Lee, Yong Jin; Cheon, Gi Jeong; Choi, Chang Woon; Lim, Sang Moo [Korea Institute of Radiological and Medical Sciences (KIRAMS), Seoul (Korea, Republic of)

    2010-09-15

    We determined the cytotoxic properties of cytochrome P450 4B1 (CYP4B1) activated 4-ipomeanol (4-ipo) and 2-aminoanthracene (2-AA) in rat glioma to verify the CYP4B1/4-ipo or 2-AA system for prodrug-activating gene therapy. The cyp4B1 cDNA was cloned into pcDNA3.1/ Hygro from rabbit lung total RNA (pcDAN-cyp4B1). Lentiviral vector encoding firefly luciferase (fLuc) was infected into C6 (rat glioma), and the fLuc-expressing cell was selected (C6-L). After transfection with pcDNA-cyp4B1 vector into C6-L, the single clone expressing cyp4B1 gene was selected (C6-CL). Prodrug for various concentrations of 4-ipo or 2-AA was treated for 72 h and 96 h. The cell survival rate of C6-CL was determined using MTT assay and trypan-blue dye exclusion methods. By RT-PCR analysis, fLuc and CYP4B1 expression was detected in C6-CL, but not in C6. MTT assay and trypan-blue dye exclusion showed that IC'5'0 of C6-CL was 0.3 mM and <0.01 mM after 4-ipo or 2-AA treatment at 96 h or 72 h exposure, respectively. Cell survivals of C6-CL were more rapidly reduced after treatment with 4-ipo or 2-AA than those of C6-L cells. The cell survival rate with MTT and trypan-blue dye exclusion assay was well correlated with fLuc activity in C6-CL cells. Conclusions CYP4B1-based prodrug-activating gene therapy may have the potential to treat glioma and the cytotoxic effects of CYP4B1 enzyme activated 4-ipo or 2-AA in C6, and could be clearly determined by bioluminescent activity in C6-CL.

  16. Crystal structure of triaqua(1,10-phenanthroline-κ2N,N′(2,4,5-trifluoro-3-methoxybenzoato-κO1cobalt(II 2,4,5-trifluoro-3-methoxybenzoate

    Directory of Open Access Journals (Sweden)

    Junshan Sun

    2014-11-01

    Full Text Available The title salt, [Co(C8H4F3O3(C12H8N2(H2O3](C8H4F3O3, was obtained under solvothermal conditions by the reaction of 2,4,5-trifluoro-3-methoxybenzoic acid with CoCl2 in the presence of 1,10-phenanthroline (phen. The CoII ion is octahedrally coordinated by two N atoms [Co—N = 2.165 (2 and 2.129 (2 Å] from the phen ligand, by one carboxylate O atom [Co—O = 2.107 (1 Å] and by three O atoms from water molecules [Co—O = 2.093 (1, 2.102 (1 and 2.114 (1 Å]. The equatorial positions of the slightly distorted octahedron are occupied by the N atoms, the carboxylate O and one water O atom. An intra- and intermolecular O—H...O hydrogen-bonding network between the water-containing complex cation and the organic anion leads to the formation of ribbons parallel to [010].

  17. (Vapour + liquid) equilibria for the binary mixtures (1-propanol + dibromomethane, or + bromochloromethane, or + 1,2-dichloroethane or + 1-bromo-2-chloroethane) at T = 313.15 K

    International Nuclear Information System (INIS)

    Gil-Hernandez, V.; Garcia-Gimenez, P.; Otin, S.; Artal, M.; Velasco, I.

    2005-01-01

    Isothermal (vapour + liquid) equilibria (VLE) at 313.15 K have been measured for liquid 1-propanol + dibromomethane, or + bromochloromethane or + 1,2-dichloroethane or + 1-bromo-2-chloroethane mixtures. The VLE data were reduced using the Redlich-Kister equation taking into consideration the vapour phase imperfection in terms of the 2nd molar virial coefficients. The excess molar Gibbs free energies of all the studied mixtures are positive and ranging from 794 J·mol -1 for (1-propanol + bromochloromethane) and 1052 J·mol -1 for (1-propanol + 1-bromo-2-chloroethane), at x = 0.5. The experimental results are compared with modified UNIFAC predictions

  18. Antipyretic action of the new hydrazides 2 - (5 - (adamantane-1-yl-4-r-1 ,2,4-triazol-3-ylthioacetate

    Directory of Open Access Journals (Sweden)

    E. S. Pruglo

    2013-06-01

    Full Text Available INTRODUCTION. It is known that fever is a necessary defense response that activates the immune system, enhances phagocytosis, stimulates the formation of Interferon, antibody production, which leads to inhibition of reproduction of many viruses and bacteria. However, the raising of the temperature above 39 ° C is dangerous for adults and children of all ages. Despite the high efficacy of analgesics, antipyretics, their use is not always safe. Therefore, the search for new highly efficient drug with antipyretic action is an urgent problem nowadays. RESEARCH GOAL - was pharmacological antipyretics screening among first synthesized derivatives of 1,2,4-triazoles. MATERIALS AND METHODS of research. The experimental fever reproduced on white nonlinear rats by administering 2,4-dinitrophenol (2,4-DNP (disconnector of the oxidative phosphorylation at a dose of 20 mg / kg. Investigated substances were injected through 0.5 hours (T 0,5 after administration of 2,4-DNP, rectal body temperature for 1 hour (T1 was fixed. Initial rectal temperature (T0 recorded to intra-abdominal injection 2.4-DNF. Acetylsalicylic acid was used as a comparison reference drug at a dose of 100 mg / kg. The results were processed with modern statistical methods of analysis on a personal computer using standard software package Microsoft Office 2010 (Microsoft Excel and «STATISTICA ® for Windows 6.0». We used 3 levels of statistical significance of differences in outcomes research - p <0.05, p <0.01, and P <0.001. RESULTS AND DISCUSSION. A new antipyretics were identified with activity not less than in the standard for comparison - acetylsalicylic acid. Intraabdominal injection of 2,4-DNF in 0.5 hour caused a fever in rat in average from 37.480 to 38.580 Co (Δ 1,10 C. Most significantly retarded the body temperature in animals compound number 76 (ΔT 1,230 C, p <0.01, 86 (ΔT 1,140 C, p <0.001, 85 (ΔT 1,330 C, p <0.01, 87 (ΔT 1,010 S , p <0.01, it’s action were somewhat

  19. Solid-phase synthesis of NH-1,2,3-triazoles using 4,4′- bismethoxybenzhydryl azide

    DEFF Research Database (Denmark)

    Cohrt, Anders Emil O'Hanlon; Le Quement, Sebastian Thordal; Nielsen, Thomas Eiland

    2014-01-01

    Readily available 4,4′-bismethoxybenzhydryl azide was found to be a useful building block for the synthesis of NH-1,2,3-triazoles through copper(I)-catalyzed cycloaddition reactions with solid-supported terminal alkynes, followed by acid-mediated deprotection. Peptide-containing NH-1,2,3-triazole...

  20. Susceptibility of 2 1/4 Cr-1Mo steel to liquid metal induced embrittlement by lithium-lead solutions

    International Nuclear Information System (INIS)

    Eberhard, B.A.; Edwards, G.R.

    1984-08-01

    An investigation has been conducted on the liquid metal induced embrittlement susceptibility of 2 1/4Cr-1Mo steel exposed to lithium and 1a/o lead-lithium at temperatures between 190 0 C and 525 0 C. This research was part of an ongoing effort to evaluate the compatibility of liquid lithium solutions with potential fusion reactor containment materials. Of particular interest was the microstructure present in a weld heat-affected zone, a microstructure known to be highly susceptible to corrosive attack by liquid lead-lithium solutions. Embrittlement susceptibility was determined by conducting tension tests on 2 1/4Cr-1Mo steel exposed to an inert environment as well as to a lead-lithium liquid and observing the change in tensile behavior. The 2 1/4Cr-1Mo steel was also given a base plate heat treatment to observe its embrittlement susceptibility to 1a/o lead-lithium. The base plate microstructure was severely embrittled at temperatures less than 500 0 C. Tempering the base plate was effective in restoring adequate ductility to the steel

  1. CERES ERBE-like Monthly Geographical Averages (ES-4) in HDF (CER_ES4_PFM+FM1_Edition1)

    Science.gov (United States)

    Wielicki, Bruce A. (Principal Investigator)

    The ERBE-like Monthly Geographical Averages (ES-4) product contains a month of space and time averaged Clouds and the Earth's Radiant Energy System (CERES) data for a single scanner instrument. The ES-4 is also produced for combinations of scanner instruments. For each observed 2.5-degree spatial region, the daily average, the hourly average over the month, and the overall monthly average of shortwave and longwave fluxes at the Top-of-the-Atmosphere (TOA) from the CERES ES-9 product are spatially nested up from 2.5-degree regions to 5- and 10-degree regions, to 2.5-, 5-, and 10-degree zonal averages, and to global monthly averages. For each nested area, the albedo and net flux are given. For each region, the daily average flux is estimated from an algorithm that uses the available hourly data, scene identification data, and diurnal models. This algorithm is 'like' the algorithm used for the Earth Radiation Budget Experiment (ERBE). The following CERES ES4 data sets are currently available: CER_ES4_FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition2 CER_ES4_PFM+FM1_Edition1 CER_ES4_PFM+FM2_Edition1 CER_ES4_TRMM-PFM_Edition1 CER_ES4_TRMM-PFM_Edition2 CER_ES4_Terra-FM1_Edition1 CER_ES4_Terra-FM2_Edition1 CER_ES4_FM1+FM2_Edition2 CER_ES4_Terra-FM1_Edition2 CER_ES4_Terra-FM2_Edition2 CER_ES4_Aqua-FM3_Edition1 CER_ES4_Aqua-FM4_Edition1 CER_ES4_FM1+FM2+FM3+FM4_Edition1 CER_ES4_Aqua-FM3_Edition2 CER_ES4_Aqua-FM4_Edition2 CER_ES4_FM1+FM3_Edition2 CER_ES4_FM1+FM4_Edition2 CER_ES4_PFM+FM1_Edition2 CER_ES4_PFM+FM2_Edition2 CER_ES4_Aqua-FM3_Edition1-CV CER_ES4_Aqua-FM4_Edition1-CV CER_ES4_Terra-FM1_Edition1-CV CER_ES4_Terra-FM2_Edition1-CV. [Location=GLOBAL] [Temporal_Coverage: Start_Date=1998-01-01; Stop_Date=2000-03-31] [Spatial_Coverage: Southernmost_Latitude=-90; Northernmost_Latitude=90; Westernmost_Longitude=-180; Easternmost_Longitude=180] [Data_Resolution: Latitude_Resolution=2.5 degree; Longitude_Resolution=2.5 degree; Horizontal

  2. CERES ERBE-like Monthly Geographical Averages (ES-4) in HDF (CER_ES4_Terra-FM1_Edition1)

    Science.gov (United States)

    Wielicki, Bruce A. (Principal Investigator)

    The ERBE-like Monthly Geographical Averages (ES-4) product contains a month of space and time averaged Clouds and the Earth's Radiant Energy System (CERES) data for a single scanner instrument. The ES-4 is also produced for combinations of scanner instruments. For each observed 2.5-degree spatial region, the daily average, the hourly average over the month, and the overall monthly average of shortwave and longwave fluxes at the Top-of-the-Atmosphere (TOA) from the CERES ES-9 product are spatially nested up from 2.5-degree regions to 5- and 10-degree regions, to 2.5-, 5-, and 10-degree zonal averages, and to global monthly averages. For each nested area, the albedo and net flux are given. For each region, the daily average flux is estimated from an algorithm that uses the available hourly data, scene identification data, and diurnal models. This algorithm is 'like' the algorithm used for the Earth Radiation Budget Experiment (ERBE). The following CERES ES4 data sets are currently available: CER_ES4_FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition2 CER_ES4_PFM+FM1_Edition1 CER_ES4_PFM+FM2_Edition1 CER_ES4_TRMM-PFM_Edition1 CER_ES4_TRMM-PFM_Edition2 CER_ES4_Terra-FM1_Edition1 CER_ES4_Terra-FM2_Edition1 CER_ES4_FM1+FM2_Edition2 CER_ES4_Terra-FM1_Edition2 CER_ES4_Terra-FM2_Edition2 CER_ES4_Aqua-FM3_Edition1 CER_ES4_Aqua-FM4_Edition1 CER_ES4_FM1+FM2+FM3+FM4_Edition1 CER_ES4_Aqua-FM3_Edition2 CER_ES4_Aqua-FM4_Edition2 CER_ES4_FM1+FM3_Edition2 CER_ES4_FM1+FM4_Edition2 CER_ES4_PFM+FM1_Edition2 CER_ES4_PFM+FM2_Edition2 CER_ES4_Aqua-FM3_Edition1-CV CER_ES4_Aqua-FM4_Edition1-CV CER_ES4_Terra-FM1_Edition1-CV CER_ES4_Terra-FM2_Edition1-CV. [Location=GLOBAL] [Temporal_Coverage: Start_Date=1998-01-01; Stop_Date=2005-10-31] [Spatial_Coverage: Southernmost_Latitude=-90; Northernmost_Latitude=90; Westernmost_Longitude=-180; Easternmost_Longitude=180] [Data_Resolution: Latitude_Resolution=2.5 degree; Longitude_Resolution=2.5 degree; Horizontal

  3. Evolution of the pi g sub 9 sub / sub 2 x nu h sub 1 sub 1 sub / sub 2 configuration in the neutron-rich sup 1 sup 1 sup 0 sup , sup 1 sup 1 sup 2 sub 4 sub 5 Rh and sup 1 sup 1 sup 4 sup , sup 1 sup 1 sup 6 sub 4 sub 7 Ag isotopes

    CERN Document Server

    Porquet, M G; Deloncle, I; Venkova, T; Astier, A; Buforn, N; Meyer, M; Prevost, A; Redon, N; Stezowski, O; Donadille, L; Dorvaux, O; Gall, B J P; Schulz, N; Lalkovski, S; Lucas, R; Minkova, A

    2003-01-01

    The sup 1 sup 1 sup 0 sup , sup 1 sup 1 sup 2 Rh and sup 1 sup 1 sup 4 sup , sup 1 sup 1 sup 6 Ag nuclei have been produced as fission fragments in the fusion reaction sup 1 sup 8 O+ sup 2 sup 0 sup 8 Pb at 85 MeV. Their level schemes have been built from gamma-rays detected using the Euroball IV array. High-spin states of these neutron-rich nuclei have been identified for the first time. The yrast structures consist of rotational bands in which the odd proton occupies the pi g sub 9 sub / sub 2 sub-shell and the odd neutron the nu h sub 1 sub 1 sub / sub 2 sub-shell. The evolution of the pi g sub 9 sub / sub 2 x nu h sub 1 sub 1 sub / sub 2 band structure is analyzed as a function of the neutron number.

  4. Preparation data of the bromodomains BRD3(1, BRD3(2, BRD4(1, and BRPF1B and crystallization of BRD4(1-inhibitor complexes

    Directory of Open Access Journals (Sweden)

    Martin Hügle

    2016-06-01

    Full Text Available This article presents detailed purification procedures for the bromodomains BRD3(1, BRD3(2, BRD4(1, and BRPF1B. In addition we provide crystallization protocols for apo BRD4(1 and BRD4(1 in complex with numerous inhibitors. The protocols described here were successfully applied to obtain affinity data by isothermal titration calorimetry (ITC and by differential scanning fluorimetry (DSF as well as structural characterizations of BRD4(1 inhibitor complexes (PDB codes: PDB: 4LYI, PDB: 4LZS, PDB: 4LYW, PDB: 4LZR, PDB: 4LYS, PDB: 5D24, PDB: 5D25, PDB: 5D26, PDB: 5D3H, PDB: 5D3J, PDB: 5D3L, PDB: 5D3N, PDB: 5D3P, PDB: 5D3R, PDB: 5D3S, PDB: 5D3T. These data have been reported previously and are discussed in more detail elsewhere [1,2].

  5. Four experimental stimulants found in sports and weight loss supplements: 2-amino-6-methylheptane (octodrine), 1,4-dimethylamylamine (1,4-DMAA), 1,3-dimethylamylamine (1,3-DMAA) and 1,3-dimethylbutylamine (1,3-DMBA).

    Science.gov (United States)

    Cohen, Pieter A; Travis, John C; Keizers, Peter H J; Deuster, Patricia; Venhuis, Bastiaan J

    2017-11-08

    The United States Food and Drug Administration banned the stimulant 1,3-dimethylamylamine (1,3-DMAA) from dietary supplements and warned consumers that the stimulant can pose cardiovascular risks ranging from high blood pressure to heart attacks. We designed our study to determine if a new stimulant similar in structure to 1,3-DMAA has been introduced as an ingredient in supplements sold in the United States (US). We analyzed six brands of supplements that listed an ingredient on the label (e.g., Aconitum kusnezoffii, DMHA or 2-amino-isoheptane) that might refer to an analog of 1,3-DMAA. Supplements were analyzed by two separate laboratories using ultra-high-performance liquid chromatography mass spectrometry and reference standards. Two previously unidentified 1,3-DMAA analogs (2-amino-6-methylheptane [octodrine] and 1,4-dimethylamylamine [1,4-DMAA]) and two banned stimulants (1,3-DMAA and 1,3-dimethylbutylamine [1,3-DMBA]) were identified. Octodrine was found at a dose (±95% CI) of 72 ± 7.5 mg per serving. In Europe, octodrine was previously sold as a pharmaceutical in multi-ingredient medications at dosages from 8 to 33 mg. The quantity of octodrine found in our study was more than twice the largest pharmaceutical dose. The other new stimulant, 1,4-DMAA, has not previously been approved for human consumption, and its safety in humans is unknown. 1,4-DMAA was found at dosages between 21 ± 11 mg to 94 ± 48 mg per serving. In addition, two banned stimulants - 1,3-DMAA and 1,3-DMBA - were also identified: 24 ± 7.6 mg to 35 ± 11 mg of 1,3-DMAA and 51 ± 16 mg of 1,3-DMBA. In one product, 24 ± 7.6 mg of 1,3-DMAA was combined with 21 ± 11 mg of 1,4-DMAA. 1,3-DMAA has been investigated as potentially contributing to hemorrhagic strokes and sudden death, whereas the safety of 1,3-DMBA in humans is unknown. Two banned stimulants (1,3-DMAA and 1,3-DMBA) and two previously unidentified stimulants (1,4-DMAA and

  6. Promising silicones modified with cationic biocides for the development of antimicrobial medical devices.

    Science.gov (United States)

    Ghamrawi, Sarah; Bouchara, Jean-Philippe; Tarasyuk, Oksana; Rogalsky, Sergiy; Lyoshina, Lyudmila; Bulko, Olga; Bardeau, Jean-François

    2017-06-01

    We have tested silicones containing 2% or 5% of the cationic biocides polyhexamethylene guanidine dodecylbenzenesulfonate (PHMG-DBS), 1-octyl-3-methylimidazolium tetrafluoroborate (OMIM-BF 4 ) or 1-dodecyl-3-methylimidazolium tetrafluoroborate (DMIM-BF 4 ) against the major relevant bacterial and yeast species in health care-associated infections (HCAI). Study conducted according to the international standard ISO 22196 revealed that silicones containing 2% or 5% DMIM-BF 4 or 5% PHMG-DBS presented the highest antimicrobial activity, leading to a logarithmic growth reduction of 3.03 to 6.46 and 3.65 to 4.85 depending on the bacterial or fungal species. Heat-pretreated silicones containing 2% DMIM-BF 4 kept a high activity, with at least a 3-log reduction in bacterial growth, except against P. aeruginosa where there was only a 1.1-log reduction. After 33days, the release ratio of cationic biocide from silicone films containing 5% of DMIM-BF 4 was found to be 5.6% in pure water and 1.9% in physiological saline solution, respectively. No leaching of PHMG-DBS polymeric biocide was detected under the same conditions. These results demonstrate unambiguously that silicones containing 2% DMIM-BF 4 or 5% PHMG-DBS present high antimicrobial activity, as well as high leaching resistance and therefore may be good candidates for the development of safer medical devices. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Quasi-1D s=1/2 antiferromagnet Cs2CuCl4 in a magnetic field

    DEFF Research Database (Denmark)

    Coldea, R.; Tennant, D.A.; Cowley, R.A.

    1997-01-01

    than the field (similar or equal to 8 T) required to fully align the spins, are observed to decouple the chains, and the system enters a disordered intermediate-field phase (IFP). The IFP excitations are in agreement with the predictions of Muller et al. for the 1D S = 1/2 HAF, and Talstra and Haldane......Magnetic excitations of the quasi-1D S = 1/2 Heisenberg antiferromagnet (HAF) Cs2CuCl4 have beer measured as a function of magnetic field using neutron scattering. For T Fields greater than B-c = 1.66 T, but less...... for the related l/r(2) chain (the Haldane-Shastry model). This behavior is inconsistent with linear spin-wave theory....

  8. 5-[(3-Fluorophenyl(2-hydroxy-6-oxocyclohex-1-en-1-ylmethyl]-6-hydroxy-1,3-dimethylpyrimidine-2,4(1H,3H-dione

    Directory of Open Access Journals (Sweden)

    Assem Barakat

    2016-09-01

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

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

    Directory of Open Access Journals (Sweden)

    Kasi Viswanatharaju Ruddraraju

    2015-04-01

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

  10. Spectral and quantum chemical studies on 1,3-bis(N(1)-4-amino-6-methoxypyrimidinebenzenesulfonamide-2,2,4,4-ethane-1,2-dithiol)-2,4-dichlorocyclodiphosph(V)azane and its erbium complex.

    Science.gov (United States)

    Al-Mogren, Muneerah M; Alaghaz, Abdel-Nasser M A; El-Gogary, Tarek M

    2014-01-24

    Novel 1,3-bis(N(1)-4-amino-6-methoxypyrimidine-benzenesulfonamide-2,2,4,4-ethane-1,2-dithiol)-2,4-dichlorocyclodiphosph(V)azane (L), was prepared and their coordinating behavior towards the lanthanide ion Er(III) was studied. The structures of the isolated products are proposed based on elemental analyses, IR, UV-VIS., (1)H NMR, (13)C NMR, (31)P NMR, SEM, XRD, mass spectra, effective magnetic susceptibility measurements and thermogravimetric analysis (TGA). Computational studies have been carried out at the DFT-B3LYP/6-31G(d) level of theory on the structural and spectroscopic properties of L and its binuclear Er(III) complex. Different tautomers of the ligand were optimized at the ab initio DFT level. Keto-form structure is about 17.7 kcal/mol more stable than the enol form (taking zpe correction into account). Simulated IR frequencies were scaled and compared with that experimentally measured. TD-DFT method was used to compute the UV-VIS spectra which compared by the measured electronic spectra. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Cation Dependence of the Dimerization Enthalpy for A2 [tetracyanoethylene]2 (A=NMe4 , Mepy, NEt4 ) Possessing a Long, Multicenter Bond.

    Science.gov (United States)

    Graham, Adora G; Fedin, Matvey V; Miller, Joel S

    2017-09-12

    [TCNE] .- (TCNE=tetracyanoethylene) has been isolated as D 2h π-[TCNE] 2 2- possessing a long, 2.9 Å multicenter 2-electron-4-center (2e - /4c) C-C bond, and as C 2 π-[TCNE] 2 2- possessing a longer, 3.04 Å multicenter 2e - /6c (4 C+2 N atoms) bond. Temperature-dependent UV/Vis spectroscopic measurements in 2-methyltetrahydrofuran (MeTHF) has led to the determination of the dimerization, 2[TCNE] .- ⇌π-[TCNE] 2 2- , equilibrium constants, K eq (T), [[TCNE] 2 2- ]/[[TCNE] .- ] 2 , enthalpy, ΔH, and entropy, ΔS, of dimerization for [Mepy] 2 [TCNE] 2 (Mepy=N-methylpyridinium, H 3 CNC 5 H 5 + ) possessing D 2h π-[TCNE] 2 2- and [NMe 4 ] 2 [TCNE] 2 possessing C 2 π-[TCNE] 2 2- conformations in the solid state; however, both form D 2h π-[TCNE] 2 2- in MeTHF solution. Based on ΔH=-3.6±0.1 kcal mol -1 (-15.2 kJ mol -1 ), and ΔS=-11±1 eu (-47 J mol -1  K -1 ) and ΔH=-2.4±0.2 kcal mol -1 (-10.2 kJ mol -1 ), and ΔS=-8±1 eu (-32 J mol -1  K -1 ) in MeTHF for [NMe 4 ] 2 [TCNE] 2 and [Mepy] 2 [TCNE] 2 , respectively, the calculated K eq (298 K) are 1.6 and 1.3 m -1 , respectively. The observed K eq (145 K) are 3 and 2 orders of magnitude greater for [NMe 4 ] 2 [TCNE] 2 and [Mepy] 2 [TCNE] 2 , respectively. The K eq (130 K) is 4470, 257, ≈0.8, and ≪0.1 m -1 for [NMe 4 ] 2 [TCNE] 2 , [Mepy] 2 [TCNE] 2 , [NEt 4 ] 2 [TCNE] 2 , and [N(nBu) 4 ] 2 [TCNE] 2 , respectively, decreasing with increasing cation size. At standard conditions and below ambient temperature the equilibrium favors the dimer for the NMe 4 + and Mepy + cations. From the decreasing enthalpy, NMe 4 + >Mepy + , along with the decrease in dimer formation K eq (T) as NMe 4 + >Mepy + >NEt 4 + >N(nBu) 4 + , the dimer bond energy decreases with increasing cation size in MeTHF. This is attributed to a decrease in the [A] + ⋅⋅⋅[TCNE] - attractive interactions with increasing cation size. Solid state UV/Vis spectroscopic determinations of [NMe 4 ] 2

  12. Improved enzymatic production of phenolated glycerides through alkyl phenolate intermediate

    DEFF Research Database (Denmark)

    Yang, Zhiyong; Feddern, Vivian; Glasius, Marianne

    2011-01-01

    This work reported a novel approach for synthesis of dihydrocaffoylated glycerides, consisting of 2 steps: enzymatic synthesis of octyl dihydrocaffeate (as a synthetic intermediate) from octanol and dihydrocaffeic acid (DHCA), and enzymatic interesterification of triglycerides with octyl dihydroc......This work reported a novel approach for synthesis of dihydrocaffoylated glycerides, consisting of 2 steps: enzymatic synthesis of octyl dihydrocaffeate (as a synthetic intermediate) from octanol and dihydrocaffeic acid (DHCA), and enzymatic interesterification of triglycerides with octyl...

  13. 2-(2,4-Dichlorophenyl-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-ylacetamide

    Directory of Open Access Journals (Sweden)

    B. Narayana

    2013-01-01

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

  14. CERES ERBE-like Monthly Geographical Averages (ES-4) in HDF (CER_ES4_FM1+FM2_Edition2)

    Science.gov (United States)

    Wielicki, Bruce A. (Principal Investigator)

    The ERBE-like Monthly Geographical Averages (ES-4) product contains a month of space and time averaged Clouds and the Earth's Radiant Energy System (CERES) data for a single scanner instrument. The ES-4 is also produced for combinations of scanner instruments. For each observed 2.5-degree spatial region, the daily average, the hourly average over the month, and the overall monthly average of shortwave and longwave fluxes at the Top-of-the-Atmosphere (TOA) from the CERES ES-9 product are spatially nested up from 2.5-degree regions to 5- and 10-degree regions, to 2.5-, 5-, and 10-degree zonal averages, and to global monthly averages. For each nested area, the albedo and net flux are given. For each region, the daily average flux is estimated from an algorithm that uses the available hourly data, scene identification data, and diurnal models. This algorithm is 'like' the algorithm used for the Earth Radiation Budget Experiment (ERBE). The following CERES ES4 data sets are currently available: CER_ES4_FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition2 CER_ES4_PFM+FM1_Edition1 CER_ES4_PFM+FM2_Edition1 CER_ES4_TRMM-PFM_Edition1 CER_ES4_TRMM-PFM_Edition2 CER_ES4_Terra-FM1_Edition1 CER_ES4_Terra-FM2_Edition1 CER_ES4_FM1+FM2_Edition2 CER_ES4_Terra-FM1_Edition2 CER_ES4_Terra-FM2_Edition2 CER_ES4_Aqua-FM3_Edition1 CER_ES4_Aqua-FM4_Edition1 CER_ES4_FM1+FM2+FM3+FM4_Edition1 CER_ES4_Aqua-FM3_Edition2 CER_ES4_Aqua-FM4_Edition2 CER_ES4_FM1+FM3_Edition2 CER_ES4_FM1+FM4_Edition2 CER_ES4_PFM+FM1_Edition2 CER_ES4_PFM+FM2_Edition2 CER_ES4_Aqua-FM3_Edition1-CV CER_ES4_Aqua-FM4_Edition1-CV CER_ES4_Terra-FM1_Edition1-CV CER_ES4_Terra-FM2_Edition1-CV. [Location=GLOBAL] [Temporal_Coverage: Start_Date=1998-01-01; Stop_Date=2002-12-31] [Spatial_Coverage: Southernmost_Latitude=-90; Northernmost_Latitude=90; Westernmost_Longitude=-180; Easternmost_Longitude=180] [Data_Resolution: Latitude_Resolution=2.5 degree; Longitude_Resolution=2.5 degree; Horizontal

  15. Treatment of wastewater containing dissolved metals by extraction-flotation

    International Nuclear Information System (INIS)

    Puget, Flavia Pereira

    2002-02-01

    In this work an alternative process for treating a wastewater containing dissolved metals (uranium and zirconium) is considered. In order to develop this work, a continuous separation unit, characterized by the association of solvent extraction and liquid-liquid flotation is used. Alamina 336 (a mixture of tri-octyl and tri-decyl amines) is used as extractant in the the extraction process, carried out inward the ejector. The splitting of the amine-water emulsion formed is carried out in a continuously operated flotation column (of approximately 2.5 L volume). The solvent extraction results showed that it is possible to reach an efficiency of about 95% for the uranium and zirconium extraction, for a metal in the feed concentration of 10 ppm and for a Q fa /Q fo ratio around 200. An efficiency of about 80% is reached in the flotation column when the liquid flowrate is equal 0.05 Lmin -1 and the air flowrate is equal 3.3 Lmin -1 . (author)

  16. Assessing toxic effects of [Omim]Cl and [Omim]BF4 in zebrafish adults using a biomarker approach.

    Science.gov (United States)

    Liu, Tong; Guo, Yingying; Wang, Jinhua; Wang, Jun; Zhu, Lusheng; Zhang, Jun; Zhang, Cheng

    2016-04-01

    In the present study, the toxic effects of 1-octyl-3-methylimidazolium chloride ([Omim]Cl) and 1-octyl-3-methylimidazolium tetrafluoroborate ([Omim]BF4) on the zebrafish livers were studied at 0, 5, 10, 20, and 40 mg L(-1) on the 7th and 14th days. In addition, the concentrations of [Omim]Cl and [Omim]BF4 in the test water, the acute toxicity of the two ionic liquids (ILs), and the influence of anions on the toxicity of the ILs were evaluated. The acute toxicity test results showed 50 % lethal concentration (LC50) values of 152.3 ± 12.1 mg L(-1) for [Omim]Cl and 144.0 ± 11.4 mg L(-1) for [Omim]BF4. At the lowest concentration investigated (5 mg L(-1)), [Omim]Cl and [Omim]BF4 did not significantly affect zebrafish during the exposure period. However, the toxic effects of these substances were enhanced as dosing concentrations and exposure times were increased. Levels of reactive oxygen species (ROS) were significantly enhanced on the 7th day after 20 mg L(-1) and on the 14th day after 10 mg L(-1) of either substance was applied, resulting in oxidative damage, such as lipid peroxidation and DNA damage. The experimental results also indicated little effect of the anions on the toxicity of ILs and consistent toxic effects of [Omim]Cl and [Omim]BF4. Graphical Abstract The graphical abstract for the present study after exposure to [Omim]Cl and [Omim]BF4. The letter R represents the anions Cl(-) and BF4 (.)

  17. Mechanisms of membrane protein insertion into liposomes during reconstitution procedures involving the use of detergents. 1. Solubilization of large unilamellar liposomes (Prepared by reverse-phase evaporation) by Triton X-100 octyl glucoside, and sodium cholate

    International Nuclear Information System (INIS)

    Paternostre, M.T.; Roux, M.; Rigaud, J.L.

    1988-01-01

    The mechanisms governing the solubilization by Triton X-100, octyl glucoside, and sodium cholate of large unilamellar liposomes prepared by reverse-phase evaporation were investigated. The solubilization process is described by the three-stage model previously proposed for the detergents. In stage I, detergent monomers are incorporated into the phospholipid bilayers until they saturate the liposomes. At this point, i.e., stage II, mixed phospholipid-detergent micelles begin to form. By stage III, the lamellar to micellar transition is complete and all the phospholipids are present as mixed micelles. The turbidity of liposome preparations was systematically measured as a function of the amount of detergent added for a wide range of phospholipid concentrations. The results allowed a quantitative determination of the effective detergent to lipid molar ratios in the saturated liposomes. The monomer concentrations of the three detergents in the aqueous phase were also determined at the lamellar to micellar transitions. These transitions were also investigated by 31 P NMR spectroscopy, and complete agreement was found with turbidity measurements. Freeze-fracture electron microscopy and permeability studies in the sublytic range of detergent concentrations indicated that during stage I of solubilization detergent partitioning between the aqueous phase and the lipid bilayer greatly affects the basic permeability of the liposomes without significantly changing the morphology of the preparations. A rough approximation of the partition coefficients was derived from the turbidity and permeability data. It is concluded that when performed systematically, turbidity measurements constitute a very convenient and powerful technique for the quantitative study of the liposome solubilization process by detergents

  18. STABILITY OF HEMOGLOBIN AND ALBUMIN ADDUCTS OF NAPHTHALENE OXIDE, 1,2-NAPHTHOQUINONE, AND 1,4-NAPHTHOQUINONE

    Science.gov (United States)

    Naphthalene is an important industrial chemical, which has recently been shown to cause tumors of the respiratory tract in rodents. It is thought that one or more reactive metabolites of naphthalene, namely, naphthalene-1,2-oxide (NPO), 1,2-naphthoquinone (1,2-NPQ), and 1,4-na...

  19. Fragrance material review on 1-spiro[4.5]dec-7-en-7-yl-4-pent-1-one.

    Science.gov (United States)

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

    2013-12-01

    A toxicologic and dermatologic review of 1-spiro[4.5]dec-7-en-7-yl-4-pent-1-one when used as a fragrance ingredient is presented. 1-Spiro[4.5]dec-7-en-7-yl-4-pent-1-one is a member of the fragrance structural group Alkyl Cyclic Ketones. These fragrances can be described as being composed of an alkyl, R1, and various substituted and bicyclic saturated or unsaturated cyclic hydrocarbons, R2, in which one of the rings may include up to 12 carbons. Alternatively, R2 may be a carbon bridge of C2-C4 carbon chain length between the ketone and cyclic hydrocarbon. This review contains a detailed summary of all published and unpublished toxicology and dermatology papers that are related to this individual fragrance ingredient and is not intended as a stand-alone document. Available data for 1-spiro[4.5]dec-7-en-7-yl-4-pent-1-one were evaluated then summarized and includes acute toxicity, skin irritation, mucous membrane (eye) irritation, skin sensitization, phototoxicity, photoallergy, repeated dose, and genotoxicity data. A safety assessment of the entire Alkyl Cyclic Ketones will be published simultaneously with this document; please refer to Belsito et al. (2013) for an overall assessment of the safe use of this material and all Alkyl Cyclic Ketones in fragrances. Copyright © 2013 Elsevier Ltd. All rights reserved.

  20. 2,3-Dibromo-3-(2-bromophenyl-1-(3-phenylsydnon-4-ylpropan-1-one

    Directory of Open Access Journals (Sweden)

    Balakrishna Kalluraya

    2010-12-01

    Full Text Available In the title compound [systematic name: 2,3-dibromo-3-(2-bromophenyl-1-(5-oxido-3-phenyl-1,2,3-oxadiazol-3-ium-4-ylpropan-1-one], C17H11Br3N2O3, the oxadiazole ring is essentially planar, with a maximum deviation of 0.003 (1 Å. The –CHBr–CHBr– chain and bromophenyl ring are disordered over two sets of sites with a refined occupany ratio of 0.756 (5:0.244 (5. The central oxadiazole ring makes dihedral angles of 54.07 (11 and 13.76 (18° with the attached phenyl and the major component of the bromo-substituted benzene rings, respectively. The dihedral angle between the major and minor components of the bromophenyl rings is 13.4 (5°. In the crystal structure, molecules are connected by C—H...O hydrogen bonds, forming [010] ribbons.

  1. Expression of the tumor suppressor genes NF2, 4.1B, and TSLC1 in canine meningiomas.

    Science.gov (United States)

    Dickinson, P J; Surace, E I; Cambell, M; Higgins, R J; Leutenegger, C M; Bollen, A W; LeCouteur, R A; Gutmann, D H

    2009-09-01

    Meningiomas are common primary brain tumors in dogs; however, little is known about the molecular genetic mechanisms involved in their tumorigenesis. Several tumor suppressor genes have been implicated in meningioma pathogenesis in humans, including the neurofibromatosis 2 (NF2), protein 4.1B (4.1 B), and tumor suppressor in lung cancer-1 (TSLC1) genes. We investigated the expression of these tumor suppressor genes in a series of spontaneous canine meningiomas using quantitative real-time reverse transcription polymerase chain reaction (RT-PCR) (NF2; n = 25) and western blotting (NF2/merlin, 4.1B, TSLC1; n = 30). Decreased expression of 4.1B and TSLC1 expression on western blotting was seen in 6/30 (20%) and in 15/30 (50%) tumors, respectively, with 18/30 (60%) of meningiomas having decreased or absent expression of one or both proteins. NF2 gene expression assessed by western blotting and RT-PCR varied considerably between individual tumors. Complete loss of NF2 protein on western blotting was not seen, unlike 4.1B and TSLC1. Incidence of TSLC1 abnormalities was similar to that seen in human meningiomas, while perturbation of NF2 and 4.1B appeared to be less common than reported for human tumors. No association was observed between tumor grade, subtype, or location and tumor suppressor gene expression based on western blot or RT-PCR. These results suggest that loss of these tumor suppressor genes is a frequent occurrence in canine meningiomas and may be an early event in tumorigenesis in some cases. In addition, it is likely that other, as yet unidentified, genes play an important role in canine meningioma formation and growth.

  2. 1-(4-(6-Fluorobenzo [d] isoxazol-3-yl) piperidin-1-yl)-2-(4-(hydroxymethyl)-1H-1,2,3-triazol-1-yl) ethanone: Synthesis, spectroscopic characterization, Hirshfeld surface analysis, cytotoxic studies and docking studies

    Science.gov (United States)

    Govindhan, M.; Viswanathan, V.; Karthikeyan, S.; Subramanian, K.; Velmurugan, D.

    2017-08-01

    Compound 1-(4-(6-fluorobenzo[d] isoxazol-3-yl) piperidin-1-yl)-2-(4-(hydroxymethyl)-1H-1, 2,3-triazol-1-yl) ethanone was synthesized in good yield by using click chemistry approach with 2-azido-1-(4-(6-flurobenzo[d]isooxazol-3-yl)piperidin-1-yl)ethanone as a starting material. The synthesized compound was characterized using IR, NMR and MS studies. Thermal stability of the compound was analyzed by using TGA and DSC technique. The single crystal XRD analysis was taken part, to confirm the structure of the compound. The intercontacts in the crystal structure are analyzed using Hirshfeld surfaces computational method. Cytotoxicity of the synthesized compound was evaluated and the results were reported. The binding analysis carried out between the newly synthesized molecule with human serum albumin using fluorescence spectroscopy technique to understand the pharmacokinetics nature of the compound for further biological application. The molecular docking studies were evaluated for the compound to elucidate insights of new molecules in carrier protein.

  3. Structure of methylene chloride addition product to zirconium tetrachloride complex with 1-tert.-butyl-2,4,4-trimethyl-2-thio-trimethylsilyl-1,3,2,4-diazaphosphasilatedine

    International Nuclear Information System (INIS)

    Brusilovets, A.I.; Rusanov, Eh.B.; Chernega, A.N.

    1995-01-01

    Complex of zirconium tetrachloride with 1-tert.-butyl-2,4,4-trimethyl--2-thio-3-trimethyl-silyl-1,3,2,4-diazaphosphasilatedine interacts with methylene chloride with formation of bis[3-tert.-butyl-2,4,4-trimethyl-1--trimethylsilyl-2-chloremethylthio-1,3,2,4-diazaphosphasilatedinium] decachlorodizirconate. Specific features of crystal and molecular structure of the compound prepared have been studied by X-ray diffraction method. 21 refs.; 2 figs.; 2 tabs

  4. Synthesis, Spatial Structure and Analgesic Activity of Sodium 3-Benzylaminocarbonyl-1-methyl-2,2-dioxo-1H-2λ6,1-benzothiazin-4-olate Solvates

    Directory of Open Access Journals (Sweden)

    Igor V. Ukrainets

    2016-10-01

    Full Text Available In order to obtain and then test pharmocologically any possible conformers of the new feasible analgesic N-benzyl-4-hydroxy-1-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxamide, its 4-O-sodium salt was synthesized using two methods. X-ray diffraction study made possible to determine that, depending on the chosen synthesis conditions, the above-mentioned compound forms either monosolvate with methanol or monohydrate, where organic anion exists in the form of three different conformers. Pharmacological testing of the two known pseudo-enantiomeric forms of the original N-benzylamide and of the two solvates of its sodium salt was performed simultaneously under the same conditions and in equimolar doses. Comparison of the results obtained while studying the peculiarities of the synthesized compounds spatial structure and biological properties revealed an important structure-action relationship. In particular, it was shown that the intensity of analgesic effect of different conformational isomers of N-benzyl-4-hydroxy-1-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxamide may change considerably: while low active conformers are comparable with piroxicam, highly active conformers are more than twice as effective as meloxicam.

  5. The features of nucleophilic substitution of the nitro group in 4-alkyl-6-nitro-1,2,4-triazolo[5,1-c][1,2,4]triazines

    Directory of Open Access Journals (Sweden)

    E. N. Ulomsky

    2017-05-01

    Full Text Available The nucleophilic substitution of the nitro group of 4-alkyl-6-nitro-4,7-dihydro-1,2,4-triazolo[5,1-c][1,2,4]triazine-7-ones on the example of interactionwith morpholine was studied. It is established that under the action of excess cycloalkylimine at room temperature the unusual easy disclosure of triazine cycle with the formation of sterically hindered hydrazones occurs which are the key intermediates for further transformations. The carrying of reaction at elevated temperatures leads to the formation of products of substitution of the nitro group with the amine and also with morpholyl hydrazones which are the products of hydrolysis of amides of hydrazones and subsequent decarboxylation. Thus, the nucleophilic substitution of the nitro group in the described triazolotriazines flows through the ANRORC mechanism.

  6. 2-[3-(4-Methoxyphenyl-1-phenyl-1H-pyrazol-5-yl]phenol

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available The title compound, C22H18N2O2, was derived from 1-(2-hydroxyphenyl-3-(4-methoxyphenylpropane-1,3-dione. The central pyrazole ring forms dihedral angles of 16.83 (5, 48.97 (4 and 51.68 (4°, respectively, with the methoxyphenyl, phenyl and hydroxyphenyl rings. The crystal packing is stabilized by O—H...N hydrogen bonding.

  7. Eco-friendly PEG-based controlled release nano-formulations of Mancozeb: Synthesis and bioefficacy evaluation against phytopathogenic fungi Alternaria solani and Sclerotium rolfsii.

    Science.gov (United States)

    Majumder, Sujan; Shakil, Najam A; Kumar, Jitendra; Banerjee, Tirthankar; Sinha, Parimal; Singh, Braj B; Garg, Parul

    2016-12-01

    Controlled release (CR) nano-formulations of Mancozeb (manganese-zinc double salt of N,N-bisdithiocarbamic acid), a protective fungicide, have been prepared using laboratory-synthesized poly(ethylene glycols) (PEGs)-based functionalized amphiphilic copolymers without using any surfactants or external additives. The release kinetics of the developed Mancozeb CR formulations were studied and compared with that of commercially available 42% suspension concentrate and 75% wettable powder. Maximum amount of Mancozeb was released on 42nd day for PEG-600 and octyl chain, PEG-1000 and octyl chain, and PEG-600 and hexadecyl chain, on 35th day for PEG-1000 and hexadecyl chain, on 28th day for PEG-1500 and octyl chain, PEG-2000 and octyl chain, PEG-1500 and hexadecyl chain, and PEG-2000 and hexadecyl chain in comparison to both commercial formulations (15th day). The diffusion exponent (n value) of Mancozeb in water ranged from 0.42 to 0.62 in tested formulations. The half-release (t 1/2 ) values ranged from 17.35 to 35.14 days, and the period of optimum availability of Mancozeb ranged from 18.54 to 35.42 days. Further, the in vitro bioefficacy evaluation of developed formulations was done against plant pathogenic fungi Alternaria solani and Sclerotium rolfsii by poison food technique. Effective dose for 50% inhibition in mgL -1 (ED 50 ) values of developed formulations varied from 1.31 to 2.79 mg L -1 for A. solani, and 1.60 to 3.14 mg L -1 for S. rolfsii. The present methodology is simple, economical, and eco-friendly for the development of environment-friendly CR formulations of Mancozeb. These formulations can be used to optimize the release of Mancozeb to achieve disease control for the desired period depending upon the matrix of the polymer used. Importantly, the maximum amount of active ingredient remains available for a reasonable period after application. In addition, the developed CR formulations were found to be suitable for fungicidal applications, allowing

  8. Phytoremediation of 1,4-dioxane-containing recovered groundwater.

    Science.gov (United States)

    Ferro, Ari M; Kennedy, Jean; LaRue, James C

    2013-01-01

    The results of a pilot-scale phytoremediation study are reported in this paper. Small plots of trees established on a closed municipal waste landfill site were irrigated with recovered groundwater containing 1,4-dioxane (dioxane) and other volatile organic compounds (VOCs). The plots were managed to minimize the leaching of irrigation water, and leaching was quantified by the use of bromide tracer. Results indicated that the dioxane (2.5 microg/L) was effectively removed, probably via phytovolatilization, and that a full-scale phytoremediation system could be used. A system is now in place at the site in which the recovered groundwater can be treated using two different approaches. A physical treatment system (PTS) will be used during the winter months, and a 12 ha phytoremediation system (stands of coniferous trees) will be used during the growing season. The PTS removes VOCs using an air-stripper, and destroys dioxane using a photo-catalytic oxidation process. Treated water will be routed to the local sewer system. The phytoremediation system, located on the landfill, will be irrigated with effluent from the PTS air-stripper containing dioxane. Seasonal use of the phytoremediation system will reduce reliance on the photo-catalytic oxidation process that is extremely energy consumptive and expensive to operate.

  9. Crystal structure of (E-3-(2,4-dimethoxyphenyl-1-(1-hydroxynaphthalen-2-ylprop-2-en-1-one

    Directory of Open Access Journals (Sweden)

    Dongsoo Koh

    2014-09-01

    Full Text Available In the title compound, C21H18O4, the C=C bond of the central enone group adopts an E conformation. The dihedral angle formed by the benzene ring and the naphthalene ring system is 6.60 (2°. The methoxy groups on the benzene ring are essentially coplanar with the ring; the C—C—O—C torsion angles being 1.6 (2 and −177.1 (1°. The hydroxy group attached to the naphthalene ring is involved in an intramolecular O—H...O hydrogen bond. The relative conformation of the two double bonds in the enone group is s-cisoid. In the crystal, weak C—H...O hydrogen bonds link the molecules into chains propagating along [010].

  10. Interaction of photoactive cis(CO)-trans(I)-Ru-(4,4‧-dicarboxylate-2,2‧-bipyridine)(CO)2I2 with anatase (1 0 1) surface

    Science.gov (United States)

    Haukka, Matti; Hirva, Pipsa

    2002-06-01

    The coordination of cis(CO)-trans(I)-Ru(4,4‧-dicarboxylate-2,2‧-bipyridine)(CO)2I2 on an anatase (1 0 1) surface was investigated using a computational density functional method. The adsorbate is able to interact with the anatase surface by one or two carboxylate substituents of the bipyridine ligand. Three of the studied coordination modes involved a single carboxylate as the binding group, including monodentate (1M), bidentate chelating (1BC) and bidentate bridging (1BB) modes. The possibility of monodentate binding via both carboxylate groups in (2M) was also studied. The results showed that the multidentate binding is clearly preferred over monodentate coordination. The stability of the modes increased in the order 1M, 1BC, 1BB and 2M. The flexibility of the bipyridine ligand was found to be the key factor in the binding via two carboxylate groups.

  11. Crystal structure of bis(1,4-diazabicyclo[2.2.2]octan-1-ium thiosulfate dihydrate

    Directory of Open Access Journals (Sweden)

    Gorgui Awa Seck

    2016-03-01

    Full Text Available The crystal structure of the hydrated title salt, 2C6H13N2+·S2O32−·2H2O, contains a centrosymmetric cyclic motif of eight hydrogen-bonded molecular subunits. Two DABCOH+ cations (DABCO = 1,4-diazabicyclo[2.2.2]octane are linked to two water molecules and two thiosulfate anions via O—H...N and O—H...O hydrogen bonds, respectively. Two other water molecules close the cyclic motif through O—H...O contacts to the first two water molecules and to the two thiosulfate anions. A second pair of DABCOH+ cations is N—H...O hydrogen bonded to the two anions and is pendant to the ring. Adjacent cyclic motifs are bridged into a block-like arrangement extending along [100] through O—H...O interactions involving the second pair of water molecules and neighbouring thiosulfate anions.

  12. Vapour pressures for 1-(butoxymethoxy)butane (dibutoxymethane) and 1,1,1,2,2,3,3,4,4-nonafluoro-4-methoxybutane (methyl nonafluorobutyl ether) over the pressure range of (15–80) kPa

    International Nuclear Information System (INIS)

    Gárate, María P.; Bejarano, Arturo; Fuente, Juan C. de la

    2016-01-01

    Highlights: • Vapour pressures of two pure potential dry-cleaning solvent were measured. • Measurements were made over the temperature range of (294.6–442.7) K. • Three commonly used vapour pressure equations were fitted to the experimental data. • The parameters of Antoine and Wagner type equations were estimated. • The relative deviations (rmsd) from the three vapour-pressure equations were <0.6%. - Abstract: Saturated pressures of 1-(butoxymethoxy)butane (dibutoxymethane) and 1,1,1,2,2,3,3,4,4-nonafluoro-4-methoxybutane (methyl nonafluorobutyl ether), new potential solvents for dry-cleaning processes, were measured with a dynamic recirculation apparatus at a pressure range of (15–80) kPa, at temperatures of (390.4–442.7) K for dibutoxymethane and (294.6–322.4) K for methyl nonafluorobutyl ether. The vapour pressures were represented using the correlations of Antoine, extended Antoine and Wagner with relative root mean square deviations of, 1%, 6% and 0.6% for dibutoxymethane, and, 1%, 2% and 0.6% for methyl nonafluorobutyl ether, respectively. The experimental data of dibutoxymethane was compared with those available in literature, the result showed consistency between both data sets.

  13. Synthesis and properties of 4-alkoxy-2-[2-hydroxy-3-(4-o,m,p-halogenoaryl-1 -piperazinyl)propyl]-6-methyl-1H-pyrrolo-[3,4-c]pyridine-1,3(2H)-diones with analgesic and sedative activities.

    Science.gov (United States)

    Sladowska, Helena; Sabiniarz, Aleksandra; Szkatuła, Dominika; Filipek, Barbara; Sapa, Jacek

    2006-01-01

    Synthesis of N-substituted derivatives of 4-alkoxy-6-methyl-1H-pyrrolo[3,4-c]pyridine-1,3(2H)-diones (17-26) is described. The chlorides, containing OH group, used in the above synthesis can exist in two isomeric forms: chain (12, 14-16) and cyclic (12a, 14a-16a). All final imides studied exhibited analgesic activity in the "writhing syndrome" test which was superior than that of acetylsalicylic acid. In the "hot plate" test only two compounds (19, 20) were active as antinociceptive agents. Furthermore, all compounds tested significantly suppressed the spontaneous locomotor activity of mice.

  14. Electron transfer in DNA duplexes containing 2-methyl-1,4-naphthoquinone

    OpenAIRE

    Bergeron, François; Houde, Daniel; Hunting, Darel J.; Wagner, J. Richard

    2004-01-01

    2-Methyl-1,4-naphthoquinone (menadione, MQ) was linked to synthetic oligonucleotides and exposed to near-UV light to generate base radical cations in DNA. This model system of electron transfer induced alkali-labile breaks at GG doublets, similar to anthraquinone and metallointercalators systems. In sharp contrast to other systems, the photolysis of MQ–DNA duplexes gave interstrand cross-links and alkali-labile breaks at bases on the complementary strand opposite the MQ moiety. For sequences ...

  15. Interactions of tetracationic porphyrins with DNA and their effects on DNA cleavage

    Science.gov (United States)

    Lebedeva, Natalya Sh.; Yurina, Elena S.; Gubarev, Yury A.; Syrbu, Sergey A.

    2018-06-01

    The interaction of tetracationic porphyrins with DNA was studied using UV-Vis absorption, fluorescence spectroscopy and viscometry, and the particle sizes were determined. Аs cationic porphyrins, two isomer porphyrins, 3,3‧,3″,3‴-(5,10,15,20-Porphyrintetrayl)tetrakis(1-methylpyridinium) (TMPyP3) and 4,4‧,4″,4‴-(5,10,15,20-Porphyrintetrayl)tetrakis(1-methylpyridinium) (TMPyP4), were studied. They differ in the position of NCH3+ group in phenyl ring of the porphyrins and hence, in degree of freedom of rotation of the phenyl rings about the central macrocycle. It was found that intercalated complexes are formed at DNA/porphyrin molar ratios (R) of 2.2 and 3.9 for TMPyP3 и TMPyP4, respectively. Decreasing R up to 0.4 and 0.8 for TMPyP3 и TMPyP4, respectively, leads mainly to formation of outside complexes due to π-π stacking between the porphyrin chromophores interacting electrostatically with phosphate framework of DNA. Each type of the obtained complexes was characterized using Scatchard approach. It was ascertained that the affinity of TMPyP4 to DNA is stronger than TMPyP3, meanwhile the wedge effect of the latter is higher. The differences between the porphyrin isomers become more evident at irradiation of their complexes with DNA. It was established that irradiation of the intercalated complexes results in DNA fragmentation. In the case of TMPyP4, DNA fragments of different size are formed. The irradiation of the outside DNA/porphyrin complexes leads to cleavage of DNA (TMPyP3 and TMPyP4) and partial destruction of the complex due to photolysis of the porphyrin (TMPyP3).

  16. New Synthesis, Structure and Analgesic Properties of Methyl 1-R-4-Methyl-2,2-Dioxo-1H-2λ6,1-Benzothiazine-3-Carboxylates

    Directory of Open Access Journals (Sweden)

    Liliana Azotla-Cruz

    2017-01-01

    Full Text Available According to the principles of the methodology of bioisosteric replacements a series of methyl 1-R-4-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylates has been obtained as potential analgesics. In addition, a fundamentally new strategy for the synthesis of compounds of this chemical class involving the introduction of N-alkyl substituent at the final stage in 2,1-benzothiazine nucleus already formed has been proposed. Using nuclear magnetic resonance (NMR spectroscopy, mass spectrometry and X-ray diffraction analysis it has been proven that in the DMSO/K2CO3 system the reaction of methyl 4-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylate and alkyl halides leads to formation of N-substituted derivatives with good yields regardless of the structure of the alkylating agent. The peculiarities of NMR (1Н and 13С spectra of the compounds synthesized, their mass spectrometric behavior and the spatial structure are discussed. In N-benzyl derivative the ability to form a monosolvate with methanol has been found. According to the results of the pharmacological testing conducted on the model of the thermal tail-flick it has been determined that replacement of 4-ОН-group in methyl 1-R-4-hydroxy-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylates for the methyl group is actually bioisosteric since all methyl 1-R-4-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylates synthesized demonstrated a statistically significant analgesic effect. The majority of the substances can inhibit the thermal pain response much more effective than piroxicam in the same dose. Under the same conditions as an analgesic the N-methyl-substituted analog exceeds not only piroxicam, but more active meloxicam as well. Therefore, it deserves in-depth biological studies on other experimental models.

  17. Uranyl-organic assemblies with the macrocyclic ligand 1, 4, 8, 11-tetra-aza-cyclo-tetradecane-1, 4, 8, 11-tetraacetate (TETA)

    International Nuclear Information System (INIS)

    Thuery, Pierre

    2010-01-01

    Three uranyl ion complexes obtained from the reaction of uranyl nitrate hexahydrate and 1, 4, 8, 11-tetra-aza-cyclo-tetradecane-1, 4, 8, 11-tetraacetic acid (H 4 TETA) were characterized by their crystal structure. The centrosymmetric macrocycle, in the [3434] conformation with either carbon or nitrogen atoms as corners, is zwitterionic, with four carboxylate groups and two or four protonated nitrogen atoms. The complexes [(UO 2 ) 2 (H 2 TETA)(C 2 O 4 )(H 2 O) 2 ] (1) and [UO 2 (H 4 TETA)(H 2 O)].NO 3 .Cl (2) were synthesized under hydrothermal conditions and 1 includes additional oxalate ligands generated in situ. Both compounds are two-dimensional polymers in which the four-fold monodentate macrocyclic ligand unites either four uranyl oxalate dinuclear species (1) or isolated uranyl ions (2). Complex 3, [UO 2 (H 2 TETA)(H 2 O)].6H 2 O, was obtained at room temperature and, although it displays the same stoichiometry as 2, it differs from it by being a three-dimensional framework. Both 2 and 3 present channels containing either counter-ions or water molecules. As often observed, the water content of the low-temperature species, 3, is higher than that of the high-temperature one, 2. (author)

  18. New Mononuclear Cu(II Complexes and 1D Chains with 4-Amino-4H-1,2,4-triazole

    Directory of Open Access Journals (Sweden)

    Marinela M. Dîrtu

    2013-12-01

    Full Text Available The crystal structures of two mononuclear Cu(II NH2trz complexes [Cu(NH2trz4(H2O](AsF62 (I and [Cu(NH2trz4(H2O](PF62 (II as well as two coordination polymers [Cu(μ2-NH2trz2Cl]Cl∙H2O (III and [Cu(μ2-NH2trz2Cl] (SiF60.5∙1.5H2O (IV are presented. Cationic 1D chains with bridging bis-monodentate μ2-coordinated NH2trz and bridging μ2-coordinated chloride ligands are present in III and IV. In these coordination polymers, the Cu(II ions are strongly antiferromagnetically coupled with J = −128.4 cm−1 for III and J = −143 cm−1 for IV (H = −JΣSiSi+1, due to the nature of the bridges between spin centers. Inter-chain interactions present in the crystal structures were taken into consideration, as well as g factors, which were determined experimentally, for the quantitative modeling of their magnetic properties.

  19. Novel routes to 1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazines and 5,6,9,10,11,11a-hexahydro-8H-pyrido[1,2-a]pyrrolo[2,1-c]pyrazines.

    Science.gov (United States)

    Katritzky, Alan R; Jain, Ritu; Xu, Yong-Jiang; Steel, Peter J

    2002-11-15

    Condensation reactions of benzotriazole and 2-(pyrrol-1-yl)-1-ethylamine (1) with formaldehyde and glutaric dialdehyde, respectively, afforded intermediates 2 and 6. Subsequent nucleophilic substitutions of the benzotriazole group in 2 and 6 with Grignard reagents, sodium cyanide, and sodium borohydride gave 1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazines 3a-e, 4, 5 and 5,6,9,10,11,11a-hexahydro-8H-pyrido[1,2-a]pyrrolo[2,1-c]pyrazines 7a-c, 8, 9, respectively, in good yields.

  20. Determination of trace mercury in water based on N-octylpyridinium ionic liquids preconcentration and stripping voltammetry.

    Science.gov (United States)

    Li, Zhenhan; Xia, Shanhong; Wang, Jinfen; Bian, Chao; Tong, Jianhua

    2016-01-15

    A novel method for determination of trace mercury in water is developed. The method is performed by extracting mercury firstly with ionic liquids (ILs) and then detecting the concentration of mercury in organic media with anodic stripping voltammetry. Liquid-liquid extraction of mercury(II) ions by four ionic liquids with N-octylpyridinium cations ([OPy](+)) was studied. N-octylpyridinium tetrafluoroborate and N-octylpyridinium trifluoromethylsulfonate were found to be efficient and selective extractant for mercury. Temperature controlled dispersive liquid phase microextraction (TC-DLPME) technique was utilized to improve the performance of preconcentration. After extraction, precipitated IL was diluted by acetonitrile buffer and mercury was detected by differential pulse stripping voltammetry (DPSV) with gold disc electrode. Mercury was enriched by 17 times while interfering ions were reduced by two orders of magnitude in the organic media under optimum condition. Sensitivity and selectivity for electrochemical determination of mercury were improved by using the proposed method. Tap, pond and waste water samples were analyzed with recoveries ranging from 81% to 107% and detection limit of 0.05 μg/L. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Banana-shaped 1,2,4-oxadiazoles

    Indian Academy of Sciences (India)

    cDipartimento di Fisica and INFM, Politecnico di Torino, C. Duca degli .... with a completely different shape (see figure 4): compound 1 possesses both smectic and ... (J/g). IIa. C7H. 15. Cr–Cr1. 137.8. Cr1–N. 149.5. Cr–N. 149.8. 49.2. N–I.

  2. 1,7-Cyclization of 1-diazo-2,4-pentadiene and its heteroanalogues: DFT study

    Science.gov (United States)

    Subbotina, Julia O.; Bakulev, V. A.; Herges, R.; Fabian, W. M. F.

    1,7-Dipolar cyclizations of 1-diazo-2,4-pentadiene 1a and its heteroanalogues 1b,c and 4c were studied using density functional theory (DFT). Although the heteroanalogue 1c has an appropriate electronic structure to allow for pseudopericyclic cyclization, natural bond order (NBO) analysis has provided evidence for the electrocyclic ring closure. Magnetic criteria (anisotropy of the induced current density [ACID], nucleus-independent chemical shifts [NICS]) confirmed the pericyclic character of the located transition states 2a,c and 5c. The activation barriers for the cyclization of 1-diazo-2,4-pentadiene 1a and its aza analogues 1c, 4c are 3.3, 8.2, and 12.3 kcal/mol at the B3LYP/6-31G(d) level, respectively. The higher barrier of the 1c?3c and 4c?3c reactions compared with 1a?3a is in line with the Hammond postulate. The out-of-plane distorted geometry of the cyclic product is an additional factor arguing against a pseudopericyclic mechanism.

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

    Science.gov (United States)

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

    2008-02-01

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

  4. Conformational properties of 1,4- and 1,5-substituted 1,2,3-triazole amino acids – building units for peptidic foldamers

    KAUST Repository

    Kann, Nina; Johansson, Johan R.; Beke-Somfai, Tamá s

    2015-01-01

    © The Royal Society of Chemistry 2015. Peptidic foldamers have recently emerged as a novel class of artificial oligomers with properties and structural diversity similar to that of natural peptides, but possessing additional interesting features granting them great potential for applications in fields from nanotechnology to pharmaceuticals. Among these, foldamers containing 1,4- and 1,5-substitued triazole amino acids are easily prepared via the Cu- and Ru-catalyzed click reactions and may offer increased side chain variation, but their structural capabilities have not yet been widely explored. We here describe a systematic analysis of the conformational space of the two most important basic units, the 1,4-substitued (4Tzl) and the 1,5-substitued (5Tzl) 1,2,3-triazole amino acids, using quantum chemical calculations and NMR spectroscopy. Possible conformations of the two triazoles were scanned and their potential minima were located using several theoretical approaches (B3LYP/6-311++G(2d,2p), ωB97X-D/6-311++G(2d,2p), M06-2X/6-311++G(2d,2p) and MP2/6-311++G(2d,2p)) in different solvents. BOC-protected versions of 4Tzl and 5Tzl were also prepared via one step transformations and analyzed by 2D NOESY NMR. Theoretical results show 9 conformers for 5Tzl derivatives with relative energies lying close to each other, which may lead to a great structural diversity. NMR analysis also indicates that conformers preferring turn, helix and zig-zag secondary structures may coexist in solution. In contrast, 4Tzl has a much lower number of conformers, only 4, and these lack strong intraresidual interactions. This is again supported by NMR suggesting the presence of both extended and bent conformers. The structural information provided on these building units could be employed in future design of triazole foldamers. This journal is

  5. Synthesis of carbon-14 and carbon-13 labelled (R)-(-)2[[4-(2,6-di-1-pyrrolidinyl-4-pyrimidinyl)-1-piperazinyl]me thyl]-3,4-dihydro-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol. [Anti-asthmatic

    Energy Technology Data Exchange (ETDEWEB)

    Ackland, M.J.; Howard, M.R.; Dring, L.G. (Upjohn Laboratories-Europe, Upjohn Ltd., Crawley (United Kingdom)); Jacobsen, E.J.; Secreast, S.L. (Upjohn Co., Kalamazoo, MI (United States))

    1993-01-01

    This paper describes the synthesis and characterisation of 2[[4-(2,6-di-1-pyrrolidinyl-4-pyrimidinyl)-1-piperazinyl]-[[sup 14]C -methyl]-3,4-dihydro-2,5,7,8-tetramethyl-2H-1-benzopyran-6-ol and 2[[4-(2,6-di-1-pyrrolidinyl-4-[[sup 13]C[sub 2

  6. Attraction and antennal response of the common wasp, Vespula vulgaris (L.), to selected synthetic chemicals in New Zealand beech forests.

    Science.gov (United States)

    El-Sayed, Ashraf M; Manning, Lee-Anne; Unelius, C Rikard; Park, Kye Chung; Stringer, Lloyd D; White, Nicola; Bunn, Barry; Twidle, Andrew; Suckling, David M

    2009-09-01

    The common wasp, Vespula vulgaris (L.), and the German wasp, Vespula germanica (F.), are significant problems in New Zealand beech forests (Nothofagus spp.), adversely affecting native birds and invertebrate biodiversity. This work was undertaken to develop synthetic attractants for these species to enable more efficient monitoring and management. Seven known wasp attractants (acetic acid, butyl butyrate, isobutanol, heptyl butyrate, octyl butyrate and 2,4-hexadienyl butyrate) were field tested, and only heptyl butyrate and octyl butyrate attracted significantly higher numbers of wasps than a non-baited trap. Accordingly, a series of straight-chain esters from methyl to decyl butyrate were prepared and field tested for attraction of social wasps. Peak biological activity occurred with hexyl butyrate, heptyl butyrate, octyl butyrate and nonyl butyrate. Polyethylene bags emitting approximately 18.4-22.6 mg day(-1) of heptyl butyrate were more attractive than polyethylene bags emitting approximately 14.7-16.8 mg day(-1) of heptyl butyrate in the field. Electroantennogram (EAG) studies indicated that queens and workers of V. vulgaris had olfactory receptor neurons responding to various aliphatic butyrates. These results are the first to be reported on the EAG response and the attraction of social wasps to synthetic chemicals in New Zealand beech forests and will enable monitoring of social wasp activity in beech forests. Copyright 2009 Society of Chemical Industry.

  7. 2-([1,2,4]triazolo[1,5-c]quinazolin-2-yl-)alkyl-(alkaryl-, aryl-)-amines and their derivatives. (3Н-quinazolin-4-yliden)hydrazides (1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)alkyl-(alkaryl-, aryl-)carboxylic acids: features of synthesis, modification and ant

    OpenAIRE

    Yu. V. Martynenko; M. S. Kazunin; E. А. Selivanova; S. I. Kovalenko

    2016-01-01

    The combination of different «pharmacophore» components in one structure connected via «linker» functional groups is one of the major and justified approaches for the synthesis of new biologically active substances. In this area (3Н-quinazoline-4-yliden)hydrazides (1,3-dioxo-1,3-dihydro-2H-іsoindol-2-yl-)alkyl-(aralkyl-, aryl-)carboxylic acids are the most interesting compounds. They contain quinazoline and іsoindole fragments united through аlkyl, аlkaryl and аryl groups and furthermore can ...

  8. 1,4,8,11-Tetra[2-aryl-1-diazenyl]-1,4,8,11-tetraazacyclotetradecanes - synthesis, characterization, and x-ray crystallography of the first tetrakistriazenes to be reported

    Energy Technology Data Exchange (ETDEWEB)

    Clarke, J.D.; Vaughan, K. [Dept. of Chemistry, Saint Mary' s Univ., Halifax, Nova Scotia (Canada)], E-mail: keith.vaughan@smu.ca; Bertolasi, V. [Dipartimento di Chimica and Centro di Strutturistica Diffrattometrica, Universita' di Ferrara, Ferrara (Italy)

    2006-10-15

    The reactions of a series of arene diazonium salts with 1,4,8,11-tetraazacyclotetradecane (cyclam) afford the novel compounds, the 1,4,8,11-tetra[2-aryl-1-diazenyl]-1,4,8,11-tetraazacyclotetradecanes (1a-1f), which are the first examples of tetrakistriazenes to be reported. The tetrakistriazenes were characterized by IR spectroscopy, proton and carbon NMR, elemental analysis, high resolution electrospray mass spectrometry, and X-ray crystallography. The analogous reaction of a diazonium salt with 1,4,7-triazacyclononane or 1,5,9-triazacyclododecane yields the tristriazenes 2, 3a, and 3b. The structures of compounds 1c and 1e were solved by X-ray crystallography at low temperature (150 K). Both molecules display a conformation where the four phenyltriazenyl groups point alternately upwards and downwards with respect to the mean macrocyclic plane. (author)

  9. 1,4,8,11-Tetra[2-aryl-1-diazenyl]-1,4,8,11-tetraazacyclotetradecanes - synthesis, characterization, and x-ray crystallography of the first tetrakistriazenes to be reported

    International Nuclear Information System (INIS)

    Clarke, J.D.; Vaughan, K.; Bertolasi, V.

    2006-01-01

    The reactions of a series of arene diazonium salts with 1,4,8,11-tetraazacyclotetradecane (cyclam) afford the novel compounds, the 1,4,8,11-tetra[2-aryl-1-diazenyl]-1,4,8,11-tetraazacyclotetradecanes (1a-1f), which are the first examples of tetrakistriazenes to be reported. The tetrakistriazenes were characterized by IR spectroscopy, proton and carbon NMR, elemental analysis, high resolution electrospray mass spectrometry, and X-ray crystallography. The analogous reaction of a diazonium salt with 1,4,7-triazacyclononane or 1,5,9-triazacyclododecane yields the tristriazenes 2, 3a, and 3b. The structures of compounds 1c and 1e were solved by X-ray crystallography at low temperature (150 K). Both molecules display a conformation where the four phenyltriazenyl groups point alternately upwards and downwards with respect to the mean macrocyclic plane. (author)

  10. catena-Poly[[[aquasilver(I]-μ-1,1′-(butane-1,4-diyldi-1H-imidazole-κ2N3:N3′] hemi(biphenyl-4,4′-dicarboxylate dihydrate

    Directory of Open Access Journals (Sweden)

    Zheyu Zhang

    2009-12-01

    Full Text Available In the title compound, {[Ag(C10H14N4(H2O](C14H8O40.5·2H2O}n, the AgI ion is three-coordinated by two N atoms from two independent 1,1′-(butane-1,4-diyldi-1H-imidazole (BBI ligands and one water O atom in a distorted T-shaped coordination geometry. The biphenyl-4,4′-dicarboxylate (BPDC dianions do not coordinate to AgI ions but act as counter-ions. The AgI ions are linked by BBI ligands, forming a zigzag chain. These chains are linked into a two-dimensional supramolecular architecture by O—H...O hydrogen-bonding interactions between water molecules and carboxylate O atoms of the BPDC dianions.

  11. 4-Fluoro-N-methyl-N-(1,2,3,4-tetrahydrocarbazol-3-ylbenzenesulfonamide

    Directory of Open Access Journals (Sweden)

    Kaspar Gothardt Rasmussen

    2009-04-01

    Full Text Available In the title compound, C19H19FN2O2S, the hydrogenated six-membered ring of the carbazole unit adopts a half-chair conformation and the plane of the fluorophenyl ring forms a dihedral angle of 41.5 (1° with respect to the carbazole mean plane. The crystal structure is segregated into layers containing the carbazole units and fluorophenyl rings in alternate (200 planes. The carbazole units form centrosymmetric face-to-face interactions [interplanar separation = 4.06 (1 Å] and edge-to-face interactions in which the N—H group is directed towards an adjacent carbazole face, with a shortest H...C contact of 2.53 Å. The fluorophenyl rings form face-to-face contacts with an approximate interplanar separation of 3.75 Å and a centroid–centroid distance of 4.73 (1 Å.

  12. CERES ERBE-like Monthly Geographical Averages (ES-4) in HDF (CER_ES4_FM1+FM4_Edition2)

    Science.gov (United States)

    Wielicki, Bruce A. (Principal Investigator)

    The ERBE-like Monthly Geographical Averages (ES-4) product contains a month of space and time averaged Clouds and the Earth's Radiant Energy System (CERES) data for a single scanner instrument. The ES-4 is also produced for combinations of scanner instruments. For each observed 2.5-degree spatial region, the daily average, the hourly average over the month, and the overall monthly average of shortwave and longwave fluxes at the Top-of-the-Atmosphere (TOA) from the CERES ES-9 product are spatially nested up from 2.5-degree regions to 5- and 10-degree regions, to 2.5-, 5-, and 10-degree zonal averages, and to global monthly averages. For each nested area, the albedo and net flux are given. For each region, the daily average flux is estimated from an algorithm that uses the available hourly data, scene identification data, and diurnal models. This algorithm is 'like' the algorithm used for the Earth Radiation Budget Experiment (ERBE). The following CERES ES4 data sets are currently available: CER_ES4_FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition1 CER_ES4_PFM+FM1+FM2_Edition2 CER_ES4_PFM+FM1_Edition1 CER_ES4_PFM+FM2_Edition1 CER_ES4_TRMM-PFM_Edition1 CER_ES4_TRMM-PFM_Edition2 CER_ES4_Terra-FM1_Edition1 CER_ES4_Terra-FM2_Edition1 CER_ES4_FM1+FM2_Edition2 CER_ES4_Terra-FM1_Edition2 CER_ES4_Terra-FM2_Edition2 CER_ES4_Aqua-FM3_Edition1 CER_ES4_Aqua-FM4_Edition1 CER_ES4_FM1+FM2+FM3+FM4_Edition1 CER_ES4_Aqua-FM3_Edition2 CER_ES4_Aqua-FM4_Edition2 CER_ES4_FM1+FM3_Edition2 CER_ES4_FM1+FM4_Edition2 CER_ES4_PFM+FM1_Edition2 CER_ES4_PFM+FM2_Edition2 CER_ES4_Aqua-FM3_Edition1-CV CER_ES4_Aqua-FM4_Edition1-CV CER_ES4_Terra-FM1_Edition1-CV CER_ES4_Terra-FM2_Edition1-CV. [Location=GLOBAL] [Temporal_Coverage: Start_Date=1998-01-01; Stop_Date=2005-03-31] [Spatial_Coverage: Southernmost_Latitude=-90; Northernmost_Latitude=90; Westernmost_Longitude=-180; Easternmost_Longitude=180] [Data_Resolution: Latitude_Resolution=2.5 degree; Longitude_Resolution=2.5 degree; Horizontal

  13. Nuclear inelastic scattering and density functional theory studies of a one-dimensional spin crossover [Fe(1,2,4-triazole)2(1,2,4-triazolato)](BF4) molecular chain.

    Science.gov (United States)

    Jenni, Kevin; Scherthan, Lena; Faus, Isabelle; Marx, Jennifer; Strohm, Cornelius; Herlitschke, Marcus; Wille, Hans-Christian; Würtz, Peter; Schünemann, Volker; Wolny, Juliusz A

    2017-07-26

    Nuclear inelastic scattering (NIS) experiments have been performed in order to study the vibrational dynamics of the low- and high-spin states of the polynuclear 1D spin crossover compound [Fe(1,2,4-triazole) 2 (1,2,4-triazolato)](BF 4 ) (1). Density functional theory (DFT) calculations using the functional B3LYP* and the basis set CEP-31G for heptameric and nonameric models of the compound yielded the normal vibrations and electronic energies for high-spin and low-spin isomers of three models differing in the distribution of anionic trz - ligands and BF 4 - anions. On the basis of the obtained energies a structural model with a centrosymmetric Fe(trzH) 4 (trz - ) 2 coordination core of the mononuclear unit of the chain is proposed. The obtained distribution of the BF 4 - counteranions in the proposed structure is similar to that obtained on the basis of X-ray powder diffraction studies by Grossjean et al. (Eur. J. Inorg. Chem., 2013, 796). The NIS data of the system diluted to 10% Fe(ii) content in a 90% Zn(ii) matrix (compound (2)) show a characteristic change of the spectral pattern of the low-spin centres, compared to the low-spin phase of the parent Fe(ii) complex (1). DFT calculations reveal that this is caused by a change of the structure of the neighbours of the low-spin centres. The spectral pattern of the high-spin centres in (2) is within a good approximation identical to that of the high-spin Fe(ii) isomer of (1). The inspection of the molecular orbitals of the monomeric model systems of [Fe(trzH) 4 (trz - ) 2 ] and [Fe(trzH) 6 ], together with calculations of spin transition energies, point towards the importance of an electrostatic effect caused by the negatively charged ligands. This results in the stabilisation of the low-spin state of the complex containing the anionic ligand and shortening of the Fe-N(trz - ) compared to the Fe-N(trzH) bond in high-spin, but not in low-spin [Fe(trzH) 4 (trz - ) 2 ].

  14. Comparative analyses of two thermophilic enzymes exhibiting both beta-1,4 mannosidic and beta-1,4 glucosidic cleavage activities from Caldanaerobius polysaccharolyticus.

    Science.gov (United States)

    Han, Yejun; Dodd, Dylan; Hespen, Charles W; Ohene-Adjei, Samuel; Schroeder, Charles M; Mackie, Roderick I; Cann, Isaac K O

    2010-08-01

    The hydrolysis of polysaccharides containing mannan requires endo-1,4-beta-mannanase and 1,4-beta-mannosidase activities. In the current report, the biochemical properties of two endo-beta-1,4-mannanases (Man5A and Man5B) from Caldanaerobius polysaccharolyticus were studied. Man5A is composed of an N-terminal signal peptide (SP), a catalytic domain, two carbohydrate-binding modules (CBMs), and three surface layer homology (SLH) repeats, whereas Man5B lacks the SP, CBMs, and SLH repeats. To gain insights into how the two glycoside hydrolase family 5 (GH5) enzymes may aid the bacterium in energy acquisition and also the potential application of the two enzymes in the biofuel industry, two derivatives of Man5A (Man5A-TM1 [TM1 stands for truncational mutant 1], which lacks the SP and SLH repeats, and Man5A-TM2, which lacks the SP, CBMs, and SLH repeats) and the wild-type Man5B were biochemically analyzed. The Man5A derivatives displayed endo-1,4-beta-mannanase and endo-1,4-beta-glucanase activities and hydrolyzed oligosaccharides with a degree of polymerization (DP) of 4 or higher. Man5B exhibited endo-1,4-beta-mannanase activity and little endo-1,4-beta-glucanase activity; however, this enzyme also exhibited 1,4-beta-mannosidase and cellodextrinase activities. Man5A-TM1, compared to either Man5A-TM2 or Man5B, had higher catalytic activity with soluble and insoluble polysaccharides, indicating that the CBMs enhance catalysis of Man5A. Furthermore, Man5A-TM1 acted synergistically with Man5B in the hydrolysis of beta-mannan and carboxymethyl cellulose. The versatility of the two enzymes, therefore, makes them a resource for depolymerization of mannan-containing polysaccharides in the biofuel industry. Furthermore, on the basis of the biochemical and genomic data, a molecular mechanism for utilization of mannan-containing nutrients by C. polysaccharolyticus is proposed.

  15. Modulation of Kir4.1 and Kir4.1-Kir5.1 channels by extracellular cations

    DEFF Research Database (Denmark)

    Søe, Rikke; Andreasen, Mogens; Klærke, Dan Arne

    2009-01-01

    This work demonstrates that extracellular Na(+) modulates the cloned inwardly rectifying K(+) channels Kir4.1 and Kir4.1-Kir5.1. Whole-cell patch clamp studies on astrocytes have previously indicated that inward potassium currents are regulated by external Na(+). We expressed Kir4.1 and Kir4.1-Kir5.......1 in Xenopus oocytes to disclose if Kir4.1 and/or Kir4.1-Kir5.1 at the molecular level are responsible for the observed effect of [Na(+)](o) and to investigate the regulatory mechanism of external cations further. Our results showed that Na(+) has a biphasic modulatory effect on both Kir4.1 and Kir4.1-Kir5.......1 currents. Depending on the Na(+)-concentration and applied voltage, the inward Kir4.1/Kir4.1-Kir5.1 currents are either enhanced or reduced by extracellular Na(+). The Na(+) activation was voltage-independent, whereas the Na(+)-induced reduction of the Kir4.1 and Kir4.1-Kir5.1 currents was both...

  16. Improving the Performances of Poly(vinylphosphonic acid) by Compositing or Copolymerization with Poly(4-(α-methyl)vinyl-1H-1,2,3-triazole)

    International Nuclear Information System (INIS)

    Han, Shuaiyuan; Yue, Baohua; Yan, Liuming

    2014-01-01

    Graphical abstract: - Highlights: • Poly(4-(α-methyl)vinyl-1H-1,2,3-triazole) is synthesized • PVPA/PMVTri polymeric composite proton conducting membranes are prepared • The proton conductivity of PVPA is improved by compositing with PMVTri • The water resistance of PVPA is improved by compositing with PMVTri • The oxidative stability is greatly improved - Abstract: The poly(vinylphosphonic acid) (PVPA), poly(4-(α-methyl)vinyl-1H-1,2,3-triazole) (PMVTri), and poly(VPA-co-MVTri) were synthesized, and proton exchange membranes were prepared based on the acid-base polymeric composite of PVPA and PMVTri, and acid-base amphoteric copolymer of poly(VPA-co-MVTri). The overall performances of PVPA, proton conductivity, thermal and oxidative stability, and water resistance, are greatly improved by compositing of PMVTri or copolymerization with 4-(α-methyl)vinyl-1H-1,2,3-triazole (MVTri). About four or eight folds improvement in maximum proton conductivity was observed in the polymeric composite of PVPA/PMVTri or acid-base amphoteric copolymer poly(VPA-co-MVTri) because of the redistribution of ions in the heterostructures of PVPA and PMVTri, respectively, compared with the pristine PVPA. At the same time, the oxidative stability and the water resistance of PVPA were also greatly improved attributing to the absent of α-H in the main chain of PMVTri and the acid-base interaction between the phosphonic acid groups and the triazolyl groups, respectively

  17. BIODEGRADATION OF DDT [1,1,1-TRICHLORO-2,2-BIS(4- CHLOROPHENYL) ETHANE] BY THE WHITE ROT FUNGUS PHANEROCHAETE CHRYSOSPORIUM

    Science.gov (United States)

    Extensive biodegradation of 1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane (DDT) by the white rot fungus Phanerochaete chrysosporium was demonstrated by disappearance and mineralization of [14C]DDT in nutrient nitrogen-deficient cultures. Mass balance studies demonstrated the form...

  18. Synthesis and characterization of new class of ionic liquids containing phenolate anion

    International Nuclear Information System (INIS)

    Lethesh, Kallidanthiyil Chellappan; Wilfred, Cecilia Devi; Taha, M. F.; Thanabalan, M.

    2014-01-01

    In these manuscript novel ionic liquids containing a new class of 'phenolate' anions was synthesized and characterized. 1-methylmidazole with different alkyl chains such as butyl, hexyl and octyl groups was used as the cationic part. All the ionic liquids were obtained as liquids at room temperature. The synthesized ionic liquids were characterized using 1 H NMR and 13 C NMR spectroscopy. The thermal stability of the ionic liquids was studied using thermo gravimetric analysis (TGA). The effect of temperature on the density and viscosity of the ionic liquids were studied over a temperature range from 293.15 K to 373.15K at atmospheric pressure. From the experimental values of density, the molecular volume, standard molar entropy and the lattice energy of the ionic liquids were calculated

  19. Synthesis and characterization of new class of ionic liquids containing phenolate anion

    Energy Technology Data Exchange (ETDEWEB)

    Lethesh, Kallidanthiyil Chellappan, E-mail: lethesh.chellappan@petronas.com.my [PETRONAS Ionic Liquids Center, Universiti Teknologi PETRONAS (Malaysia); Wilfred, Cecilia Devi; Taha, M. F. [Department of Chemical Engineering, Universiti Teknologi PETRONAS (Malaysia); Thanabalan, M. [Fundamental and Applied Sciences, Universiti Teknologi PETRONAS (Malaysia)

    2014-10-24

    In these manuscript novel ionic liquids containing a new class of 'phenolate' anions was synthesized and characterized. 1-methylmidazole with different alkyl chains such as butyl, hexyl and octyl groups was used as the cationic part. All the ionic liquids were obtained as liquids at room temperature. The synthesized ionic liquids were characterized using {sup 1}H NMR and {sup 13}C NMR spectroscopy. The thermal stability of the ionic liquids was studied using thermo gravimetric analysis (TGA). The effect of temperature on the density and viscosity of the ionic liquids were studied over a temperature range from 293.15 K to 373.15K at atmospheric pressure. From the experimental values of density, the molecular volume, standard molar entropy and the lattice energy of the ionic liquids were calculated.

  20. 2-Methylsulfanyl-5,6-dihydro-2H-1,3-dithiolo[4,5-b][1,4]dioxin-2-ium tetrafluoroborate

    Directory of Open Access Journals (Sweden)

    Guoquan Zhou

    2012-04-01

    Full Text Available The title compound, C6H7O2S3+·BF4−, consists of a planar 2-thioxo-1,3-dithiol-4,5-yl unit [maximum deviation from the ring plane = 0.020 (3 Å], with an ethylenedioxy group fused at the 4,5-positions; the ethylenedioxy C atoms are disordered over two positions with site-occupancy factors of 0.5. The 1,4-dioxine ring has a twist-chair conformation. Weak cation–anion S...F interactions [3.022 (4–3.095 (4 Å] and an S...O [3.247 (4 Å] interaction are present.

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

    Science.gov (United States)

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

    2010-03-01

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

  2. Synthesis and Antimicrobial Activities of Some New 1,2,4-Triazole Derivatives

    Directory of Open Access Journals (Sweden)

    Hakan Bektaş

    2010-04-01

    Full Text Available Some novel 4,5-disubstituted-2,4-dihydro-3H-1,2,4-triazol-3-one (3, 6, 8, 9 derivatives and or 3-(4-methylphenyl[1,2,4]triazolo[3,4-b][1,3]benzoxazole (5 were synthesized from the reaction of various ester ethoxycarbonylhydrazones (1a-e with several primary amines. The synthesis of 4-amino-5-(4-chlorophenyl-2-[(5-mercapto-1,3,4-oxadiazol-2-ylmethyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (13 was performed starting from 4-Amino-5-(4-chlorophenyl-2,4-dihydro-3H-1,2,4-triazol-3-one (2 by four steps; then 13 was converted to the corresponding Schiff base (14 by using 4-methoxybenzaldehyde. Finally, two Mannich base derivatives of 14 were obtained by using morpholine or methyl piperazine as amine component. All newly synthesized compounds were screened for their antimicrobial activities and some of which were found to possess good or moderate activities against the test microorganisms.

  3. (3,4-dihydroisoquinolin-2(1H)-yl)

    Indian Academy of Sciences (India)

    Administrator

    HIV-1 reverse transcriptase (HIV-1 RT); non-nucleoside reverse transcriptase inhibitor. (NNRTI); docking; autodock; 1,2,3,4-tetrahydroisoquinoline. 1. Introduction. Acquired immuno deficiency syndrome (AIDS) is one of the most serious pandemic public health chal- lenges since 1981. 1. Human immuno deficiency virus.

  4. Structural and electrochemical studies of TiO2 complexes with (4,4'-((1E,1'E)-(2,5-bis(octyloxy)-1,4-phenylene)bis(ethene-2,1-diyl))bis-(E)-N-(2,5-bis(octyloxy)benzylidene)) imine derivative bases towards organic devices.

    Science.gov (United States)

    Rozycka, Anna; Iwan, Agnieszka; Bogdanowicz, Krzysztof Artur; Filapek, Michal; Górska, Natalia; Hreniak, Agnieszka; Marzec, Monika

    2018-06-12

    Three (4,4'-((1E,1'E)-(2,5-bis(octyloxy)-1,4-phenylene)bis(ethene-2,1-diyl))bis-(E)-N-(2,5-bis(octyloxy)benzylidene)) imine derivatives were synthesized via a condensation reaction with p-toluenesulfonic acid as a catalyst. The effects of the end groups and vinylene (-HC[double bond, length as m-dash]CH-) moieties on the structural, thermal, optical, electrochemical and photovoltaic properties of imines were investigated to check the influence of TiO2 on the imine properties. The thermal behavior of imines and their complexes with TiO2 was widely investigated using FT-IR, XRD, DSC and POM methods in order to determine the order type in the imine structure. All imines present the highest occupied molecular orbital (HOMO) levels of about -5.39 eV (SAI1 and SAI2) and -5.27 eV (SAI3) and the lowest unoccupied molecular orbital (LUMO) levels at about -3.17 eV. The difference of the end groups in the imines in each case did not affect redox properties. Generally, both oxidation and reduction are easier after TiO2 addition and it also changes the HOMO-LUMO levels of imines. Moreover, changes in the characteristic bands for imines in the region 1500-1700 cm-1 observed as a drastic decrease of intensity or even disappearance of bands in the imine : TiO2 mixture suggest the formation of a complex (C[double bond, length as m-dash]N)-TiO2. Organic devices with the configuration of ITO/TiO2/SAIx (or SAIx : TiO2)/Au were fabricated and investigated in the presence and absence of visible light irradiation with an intensity of 93 mW cm-2. In all imines and complexes with TiO2, the generation of the photocurrent indicates their use as photodiodes and the best result was observed for SAI3 : TiO2 complexes.

  5. Experimental infection of clade 1.1.2 (H5N1), clade 2.3.2.1c (H5N1) and clade 2.3.4.4 (H5N6) highly pathogenic avian influenza viruses in dogs.

    Science.gov (United States)

    Lyoo, K S; Na, W; Phan, L V; Yoon, S W; Yeom, M; Song, D; Jeong, D G

    2017-12-01

    Since the emergence of highly pathogenic avian influenza (HPAI) H5N1 in Asia, the haemagglutinin (HA) gene of this virus lineage has continued to evolve in avian populations, and H5N1 lineage viruses now circulate concurrently worldwide. Dogs may act as an intermediate host, increasing the potential for zoonotic transmission of influenza viruses. Virus transmission and pathologic changes in HPAI clade 1.1.2 (H5N1)-, 2.3.2.1c (H5N1)- and 2.3.4.4 (H5N6)-infected dogs were investigated. Mild respiratory signs and antibody response were shown in dogs intranasally infected with the viruses. Lung histopathology showed lesions that were associated with moderate interstitial pneumonia in the infected dogs. In this study, HPAI H5N6 virus replication in dogs was demonstrated for the first time. Dogs have been suspected as a "mixing vessel" for reassortments between avian and human influenza viruses to occur. The replication of these three subtypes of the H5 lineage of HPAI viruses in dogs suggests that dogs could serve as intermediate hosts for avian-human influenza virus reassortment if they are also co-infected with human influenza viruses. © 2017 Blackwell Verlag GmbH.

  6. Crystal structure of 1-{3-(4-methylphenyl-5-[(E-2-phenylethenyl]-4,5-dihydro-1H-pyrazol-1-yl}ethan-1-one

    Directory of Open Access Journals (Sweden)

    Farook Adam

    2015-12-01

    Full Text Available The title compound, C20H20N2O, was studied as a part of our work on pyrazoline derivatives. It represents a trans-isomer. The central pyrazoline ring adopts an envelope conformation with the asymmetric C atom having the largest deviation of 0.107 (1 Å from the mean plane. It forms dihedral angles of 6.2 (1 and 86.4 (1° with the adjacent p-tolyl and styrene groups, respectively. In the crystal, C—H...O interactions link molecules into infinite chains along the c axis.

  7. 4-(2-Chloro-4-methoxy-5-methylphenyl)-N-[(1S)-2-cyclopropyl-1-(3-fluoro-4-methylphenyl)ethyl]5-methyl-N-(2-propynyl)-1,3-thiazol-2-amine hydrochloride (SSR125543A): a potent and selective corticotrophin-releasing factor(1) receptor antagonist. I. Biochemical and pharmacological characterization.

    Science.gov (United States)

    Gully, Danielle; Geslin, Michel; Serva, Laurence; Fontaine, Evelyne; Roger, Pierre; Lair, Christine; Darre, Valerie; Marcy, Claudine; Rouby, Pierre-Eric; Simiand, Jacques; Guitard, Josette; Gout, Georgette; Steinberg, Regis; Rodier, Daniel; Griebel, Guy; Soubrie, Philippe; Pascal, Marc; Pruss, Rebecca; Scatton, Bernard; Maffrand, Jean-Pierre; Le Fur, Gerard

    2002-04-01

    4-(2-Chloro-4-methoxy-5-methylphenyl)-N-[(1S)-2-cyclopropyl-1- (3-fluoro-4-methylphenyl)ethyl]5-methyl-N-(2-propynyl)-1,3-thiazol-2-amine hydrochloride (SSR125543A), a new 2-aminothiazole derivative, shows nanomolar affinity for human cloned or native corticotrophin-releasing factor (CRF)(1) receptors (pK(i) values of 8.73 and 9.08, respectively), and a 1000-fold selectivity for CRF(1) versus CRF(2 alpha) receptor and CRF binding protein. SSR125543A antagonizes CRF-induced stimulation of cAMP synthesis in human retinoblastoma Y 79 cells (IC(50) = 3.0 +/- 0.4 nM) and adrenocorticotropin hormone (ACTH) secretion in mouse pituitary tumor AtT-20 cells. SSR125543A is devoid of agonist activity in these models. Its brain penetration was demonstrated in rats by using an ex vivo [(125)I-Tyr(0)] ovine CRF binding assay. SSR125543A displaced radioligand binding to the CRF(1) receptor in the brain with an ID(50) of 6.5 mg/kg p.o. (duration of action >24 h). SSR125543A also inhibited the increase in plasma ACTH levels elicited in rats by i.v. CRF (4 microg/kg) injection (ID(50) = 1, 5, or 5 mg/kg i.v., i.p., and p.o., respectively); this effect lasted for more than 6 h when the drug was given orally at a dose of 30 mg/kg. SSR125543A (10 mg/kg p.o.) reduced by 73% the increase in plasma ACTH levels elicited by a 15-min restraint stress in rats. Moreover, SSR125543A (20 mg/kg i.p.) also antagonized the increase of hippocampal acetylcholine release induced by i.c.v. injection of 1 microg of CRF in rats. Finally, SSR125543A reduced forepaw treading induced by i.c.v. injection of 1 microg of CRF in gerbils (ID(50) = approximately 10 mg/kg p.o.). Altogether, these data indicate that SSR125543A is a potent, selective, and orally active CRF(1) receptor antagonist.

  8. Photostability and efficacy studies of topical formulations containing UV-filters combination and vitamins A, C and E.

    Science.gov (United States)

    Gaspar, L R; Campos, P M B G Maia

    2007-10-01

    It is already known that the photostability of a sunscreen is important for its performance on human skin. On the other hand, there are many formulations besides sunscreens containing combinations of UV-filters and daily use active substances with other claims like hydration and anti-aging effects. Vitamins A, C and E are frequently added in these kinds of products and it is not known if the UV-filters have some influence on the hydration and anti-aging effects of these vitamins on the skin as well as on their stability mainly when photounstable UV-filters like avobenzone and octyl methoxycinnamate are present in the formulation. Thus, the aim of this study was to evaluate the influence of two different UV-filters combinations, a photostable and a photounstable one, on the photostability as well as on the efficacy of a formulation containing vitamin A, C and E derivatives. The formulations that were investigated contained or not (vehicle: formulation 1) a combination of 0.6 % (w/w) vitamin A palmitate (1,700,000 UI/g), 2 % (w/w) vitamin E acetate and 2% (w/w) ascorbyl tetraisopalmitate (formulation 2) supplemented with a photounstable UV filter combination octyl methoxycinnamate (OMC), avobenzone (AVB) and 4-methylbenzilidene camphor (MBC) (formulation 3) or with a photostable UV filter combination OMC, benzophenone-3 (BP-3) and octocrylene (OC) (formulation 4). In the photostability studies, all formulations were spread onto a glass plate and exposed to UVA/UVB irradiation. The filter components and vitamins were quantified by HPLC analysis with detection at 325 and 235 nm and by spectrophotometry. To simulate the effects of these formulations daily use, all of them (formulations 1-4) were applied on the dorsum of hairless mice, which were submitted to a controlled light-dark cycle (and were not irradiated), once a day for 5 days. Transepidermal water loss (TEWL), water content of the stratum corneum and viscoelastic properties of the skin were analyzed by using

  9. Improved high-voltage performance of LiNi1/3Co1/3Mn1/3O2 cathode with Tris(2,2,2-trifluoroethyl) phosphite as electrolyte additive

    International Nuclear Information System (INIS)

    Wang, Long; Ma, Yulin; Li, Qin; Cui, Yingzhi; Wang, Panpan; Cheng, Xinqun; Zuo, Pengjian; Du, Chunyu; Gao, Yunzhi

    2017-01-01

    Tris(2,2,2-trifluoroethyl) phosphite (TTFEP) is investigated as an electrolyte additive to improve the electrochemical performance of LiNi 1/3 Co 1/3 Mn 1/3 O 2 cathode at high operating voltage (4.6 V). Charge/discharge measurements demonstrate that TTFEP is effective to improve the cycling stability and rate capability of LiNi 1/3 Co 1/3 Mn 1/3 O 2 cathode. The capacity retention of LiNi 1/3 Co 1/3 Mn 1/3 O 2 /Li cell with 1% TTFEP-containing electrolyte reaches up to 85.4% after 100 cycles at 0.5C (1C = 160 mA g −1 ), while that of the cell with the baseline electrolyte (1 M LiPF 6 in EC/DMC electrolyte) only remains 74.2%. Moreover, the discharge capacity of the cathode with 1% TTFEP-containing electrolyte could maintain around 112.0 mAh g −1 at 4C. Based on the characterization of electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS), a protective interphase film formed on the cathode surface can be found due to the preferential oxidation of TTFEP, which inhibits the electrolyte decomposition and mitigates the cathode structural destruction, leading to the improved electrochemical performance of LiNi 1/3 Co 1/3 Mn 1/3 O 2 cathode at high voltage.

  10. Reactions of 1-methyl-derivatives of 2-oxo-1,2,3,4-tetrahydropyrimidine with phosphorus pentachloride and phosphorus oxychloride

    International Nuclear Information System (INIS)

    Khanina, E.L.; Liepin'sh, E.E.; Mutsenietse, D.Kh.; Dubur, G.Ya.

    1987-01-01

    In the reaction of 4-phenyl-and 4,6-diphenyl-1-methyl-2-oxo-5-ethoxycarbonyl-1,2,3,4-tetrahydropyrimidines with phosphorus pentachloride, oxidation and dealkylation takes place in addition to chlorination and as a result one obtained 4-phenyl- and 4,6-diphenyl-1-methyl-5-ethoxycarbonyl-2-pyrimidones and also 4-phenyl-, (4,6-diphenyl)-5-ethoxycarbonyl-2-chloropyrimidines. 1,6-Dimethyl-2-oxo-4-phenyl-5-ethoxycarbonyl-1,2,3,4-tetrahydropyrimidine in the same reaction gives 1-methyl-2-oxo-4-phenyl-5-ethoxycarbonyl 6-dichloromethyl-1,2,3,4-tetrahydropyrimidine, together with 6-chloromethylene- and 6-dichloromethylene-1-methyl-2-oxo-4-phenyl-5-chloro-5-ethoxycarbonylhexahydropyrimidines. The structure was established on the basis of elemental analysis, proton NMR spectra, and carbon-13 NMR spectra, taking into account the long-range 2 H- 13 C coupling constants

  11. Synthesis, Structure, and Cyclocondensation of the 4,4,4-Trifluoro-3,3-dihydroxy-2-methyl-1-(thien-2-yl-1-butanone with Hydroxylamine and Hydrazine

    Directory of Open Access Journals (Sweden)

    Alex F. C. Flores

    2018-01-01

    Full Text Available The synthesis of 4,4,4-trifluoro-3,3-dihydroxy-2-methyl-1-(thien-2-ylbutan-1-one (3 through acylation of 1,1-dimethoxy-1-(thien-2-ylpropane (1 with trifluoroacetic anhydride and its reactions with hydroxylamine and hydrazine was investigated. X-ray structural analysis of new trifluoromethyl-substituted dielectrophile 3 revealed that this hydrate exists as a racemate with inter- and intramolecular O-H·O bonds. The crystal structure shows alignment along axis b of pair molecules with the same configuration of the O2-H·O1 bond. For 5(3-trifluoromethyl-4-methyl-3(5-(thien-2-yl-1H-pyrazole (4, obtained via cyclocondensation of precursor 2 and hydrazine hydrochloride, X-ray structural analysis indicated that its rings are almost planar (torsion angle N2-C5-C6-C7–5.4° and that S1 at the thienyl moiety is anti-periplanar to N2 (torsion angle N2-C5-C6-S1 176.01; no disorder effect was observed for the thienyl ring.

  12. 1,3-Di-4-pyridylpropane–4,4′-oxydibenzoic acid (1/1

    Directory of Open Access Journals (Sweden)

    Hirofumi Hinode

    2008-12-01

    Full Text Available The hydrothermal reaction of Cd(NO32·4H2O, 1,3-di-4-pyridylpropane (BPP and 4,4′-oxydibenzoic acid (OBA led to the formation of the title compound, C13H14N2·C14H10O5. The asymmetric unit consists of one molecule of OBA and one of BPP. In the OBA molecule, one COOH group is nearly planar with its attached benzene ring [dihedral angle = 0.9 (1°], while the other COOH group is slightly twisted with a dihedral angle of 10.8 (3°. The carboxyl groups form strong intermolecular O—H...N hydrogen bonds with N atoms of the pyridine rings in BPP, linking the molecules into zigzag chains.

  13. Anxiolytic-like and antidepressant-like activities of MCL0129 (1-[(S)-2-(4-fluorophenyl)-2-(4-isopropylpiperadin-1-yl)ethyl]-4-[4-(2-methoxynaphthalen-1-yl)butyl]piperazine), a novel and potent nonpeptide antagonist of the melanocortin-4 receptor.

    Science.gov (United States)

    Chaki, Shigeyuki; Hirota, Shiho; Funakoshi, Takeo; Suzuki, Yoshiko; Suetake, Sayoko; Okubo, Taketoshi; Ishii, Takaaki; Nakazato, Atsuro; Okuyama, Shigeru

    2003-02-01

    We investigated the effects of a novel melanocortin-4 (MC4) receptor antagonist,1-[(S)-2-(4-fluorophenyl)-2-(4-isopropylpiperadin-1-yl)ethyl]-4-[4-(2-methoxynaphthalen-1-yl)butyl]piperazine (MCL0129) on anxiety and depression in various rodent models. MCL0129 inhibited [(125)I][Nle(4)-D-Phe(7)]-alpha-melanocyte-stimulating hormone (alpha-MSH) binding to MC4 receptor with a K(i) value of 7.9 nM, without showing affinity for MC1 and MC3 receptors. MCL0129 at 1 microM had no apparent affinity for other receptors, transporters, and ion channels related to anxiety and depression except for a moderate affinity for the sigma(1) receptor, serotonin transporter, and alpha(1)-adrenoceptor, which means that MCL0129 is selective for the MC4 receptor. MCL0129 attenuated the alpha-MSH-increased cAMP formation in COS-1 cells expressing the MC4 receptor, whereas MCL0129 did not affect basal cAMP levels, thereby indicating that MCL0129 acts as an antagonist at the MC4 receptor. Swim stress markedly induced anxiogenic-like effects in both the light/dark exploration task in mice and the elevated plus-maze task in rats, and MCL0129 reversed the stress-induced anxiogenic-like effects. Under nonstress conditions, MCL0129 prolonged time spent in the light area in the light/dark exploration task and suppressed marble-burying behavior. MCL0129 shortened immobility time in the forced swim test and reduced the number of escape failures in inescapable shocks in the learned helplessness test, thus indicating an antidepressant potential. In contrast, MCL0129 had negligible effects on spontaneous locomotor activity, Rotarod performance, and hexobarbital-induced anesthesia. These observations indicate that MCL0129 is a potent and selective MC4 antagonist with anxiolytic- and antidepressant-like activities in various rodent models. MC4 receptor antagonists may prove effective for treating subjects with stress-related disorders such as depression and/or anxiety.

  14. Mechanochemical synthesis and crystal structure of a 1:2 co-crystal of 1,3,6,8-tetraazatricyclo[4.3.1.13,8]undecane (TATU and 4-chloro-3,5-dimethylphenol

    Directory of Open Access Journals (Sweden)

    Augusto Rivera

    2016-11-01

    Full Text Available Solvent-free treatment of 1,3,6,8-tetraazatricyclo[4.3.1.13,8]undecano (TATU with 4-chloro-3,5-dimethylphenol led to the formation of the title co-crystal, C7H14N4·2C8H9ClO. The asymmetric unit contains one aminal cage molecule and two phenol molecules linked via two O—H...N hydrogen bonds. In the aminal cage, the N–CH2–CH2–N unit is slightly distorted from a syn periplanar geometry. Aromatic π–π stacking between the benzene rings from two different neighbouring phenol molecules [centroid–centroid distance = 4.0570 (11 Å] consolidates the crystal packing.

  15. CH{sub 4} dehydrogenation on Cu(1 1 1), Cu@Cu(1 1 1), Rh@Cu(1 1 1) and RhCu(1 1 1) surfaces: A comparison studies of catalytic activity

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Riguang; Duan, Tian [Key Laboratory of Coal Science and Technology of Ministry of Education and Shanxi Province, Taiyuan University of Technology, Taiyuan 030024, Shanxi (China); Ling, Lixia [Key Laboratory of Coal Science and Technology of Ministry of Education and Shanxi Province, Taiyuan University of Technology, Taiyuan 030024, Shanxi (China); Research Institute of Special Chemicals, Taiyuan University of Technology, Taiyuan 030024, Shanxi (China); Wang, Baojun, E-mail: wangbaojun@tyut.edu.cn [Key Laboratory of Coal Science and Technology of Ministry of Education and Shanxi Province, Taiyuan University of Technology, Taiyuan 030024, Shanxi (China)

    2015-06-30

    Highlights: • Adsorbed Rh atom on Cu catalyst exhibits better catalytic activity for CH{sub 4} dehydrogenation. • The adsorbed Rh atom is the reaction active center for CH{sub 4} dehydrogenation. • The morphology of Cu substrate has negligible effect on CH{sub 4} dehydrogenation. - Abstract: In the CVD growth of graphene, the reaction barriers of the dehydrogenation for hydrocarbon molecules directly decide the graphene CVD growth temperature. In this study, density functional theory method has been employed to comparatively probe into CH{sub 4} dehydrogenation on four types of Cu(1 1 1) surface, including the flat Cu(1 1 1) surface (labeled as Cu(1 1 1)) and the Cu(1 1 1) surface with one surface Cu atom substituted by one Rh atom (labeled as RhCu(1 1 1)), as well as the Cu(1 1 1) surface with one Cu or Rh adatom (labeled as Cu@Cu(1 1 1) and Rh@Cu(1 1 1), respectively). Our results show that the highest barrier of the whole CH{sub 4} dehydrogenation process is remarkably reduced from 448.7 and 418.4 kJ mol{sup −1} on the flat Cu(1 1 1) and Cu@Cu(1 1 1) surfaces to 258.9 kJ mol{sup −1} on RhCu(1 1 1) surface, and to 180.0 kJ mol{sup −1} on Rh@Cu(1 1 1) surface, indicating that the adsorbed or substituted Rh atom on Cu catalyst can exhibit better catalytic activity for CH{sub 4} complete dehydrogenation; meanwhile, since the differences for the highest barrier between Cu@Cu(1 1 1) and Cu(1 1 1) surfaces are smaller, the catalytic behaviors of Cu@Cu(1 1 1) surface are very close to the flat Cu(1 1 1) surface, suggesting that the morphology of Cu substrate does not obviously affect the dehydrogenation of CH{sub 4}, which accords with the reported experimental observations. As a result, the adsorbed or substituted Rh atom on Cu catalyst exhibit a better catalytic activity for CH{sub 4} dehydrogenation compared to the pure Cu catalyst, especially on Rh-adsorbed Cu catalyst, we can conclude that the potential of synthesizing high-quality graphene with the

  16. Aminoacid N-substituted 1,4,7-triazacyclononane and 1,4,7,10-tetraazacyclododecane Zn2+, Cd2+ and Cu2+ complexes. A preparative, potentiometric titration and NMR spectroscopic study.

    Science.gov (United States)

    Plush, Sally E; Lincoln, Stephen F; Wainwright, Kevin P

    2004-05-07

    The pK(a)s and Zn2+, Cd2+ and Cu2+ complexation constants (K) for 1,4,7-tris[(2''S)-acetamido-2''-(methyl-3''-phenylpropionate)]-1,4,7-triazacyclononane, 1, 1,4,7-tris[(2''S)-acetamido-2''-(1''-carboxy-3''-phenylpropane)]-1,4,7-triazacyclononane, H(3)2, 1,4,7-tris[(2''S)-acetamido-2''-(methyl-3''-(1H-3-indolyl)propionate)]-1,4,7-triazacyclononane, 3, and 1,4,7,10-tetrakis[(2''S)-acetamido-2''-(methyl-3''-phenylpropionate)]-1,4,7,10-tetraazacyclododecane, 4, 1,4,7,10-tetrakis[(2''S)-acetamido-2''-(1''-carboxy-3''-phenylpropane)]-1,4,7,10-tetraazacyclododecane, H(4)5, in 20 : 80 v/v water-methanol solution are reported. The pK(a)s within the potentiometric detection range for H(3)1(3+) = 8.69 and 3.59, for H(6)2(3+) = 9.06, 6.13, 4.93 and 4.52, H(3)3(3+) = 8.79 and 3.67, H(4)4(4+) = 8.50, 5.62 and 3.77 and for H(8)5(4+) = 9.89, 7.06, 5.53, 5.46, 4.44 and 4.26 where each tertiary amine nitrogen is protonated. The complexes of 1: [Zn(1)]2+(9.00), [Cd(1)]2+ (6.49), [Cd(H1)]3+ (4.54) and [Cu(1)]2+ (10.01) are characterized by the log(K/dm3 mol(-1)) values shown in parentheses. Analogous complexes are formed by 3 and 4: [Zn(3)]2+ (10.19), [Cd(3)]2+ (8.54), [Cu(3)]2+ (10.77), [Zn(4)]2+ (11.41) [Cd(4)]2+ (9.16), [Cd(H4)]3+ (6.16) and [Cu(4)]2+ (11.71). The tricarboxylic acid H(3)2 generates a greater variety of complexes as exemplified by: [Zn(2)-] (10.68) [Zn(H2)] (6.60) [Zn(H(2)2)+] (5.15), [Cd(2)](-) (4.99), [Cd(H2)] (4.64), [Cd(H2(2))]+ (3.99), [Cd(H(3)2)]2+ (3.55), [Cu(2)](-) (12.55) [Cu(H2)] (7.66), [Cu(H(2)2)]+ (5.54) and [Cu(2)2](4-) (3.23). The complexes of H(4)5 were insufficiently soluble to study in this way. The 1H and 13C NMR spectra of the ligands are consistent with formation of a predominant Zn2+ and Cd2+ Delta or Lambda diastereomer. The preparations of the new pendant arm macrocycles H(3)2, 3, 4 and H(4)5 are reported.

  17. Autoradiography of 1-methyl-4-phenyl-1,2,3,6-tetrahydropyridine (MPTP): Uptake in the monoaminergic pathways and in melanin containing tissues

    Energy Technology Data Exchange (ETDEWEB)

    Lyden, A; Lindquist, N G; Bondesson, U; Larsson, B S; Olsson, L -I

    1985-01-01

    A recently discovered neurotoxic compound, 1-methyl-4-phenyl-1,2,3,6-tetrahydropyridine, has been found to cause a parkinsonian-like syndrome in man and monkey, but not in laboratory animals such as rat, mouse and guinea pig. MPTP seems to selectively destroy the melanin containing dopaminergic cells in pars compacta of substantia nigra. Lower mammalian species do not have melanin in these cells, which indicates that the presence of neuromelanin may be of importance for the development of MPTP-induced lesions. By means of whole-body autoradiography of TH-MPTP in mice, accumulation and retention was observed in the dopaminergic pathways, in locus ceruleus and in structures in the medulla oblongata and spinal cord. A high uptake was also seen in melanin-containing tissues such as in the eyes of pigmented mice. MPTP has earlier been found to have high affinity in vitro for dopamine melanin, which is similar to the pigment in substantia nigra. The typical features of the MPTP-induced neurotoxicity with destruction of pigmented nerve cells and development of parkinsonism may be due to accumulation adn retention of MPTP and its metabolites in these cells. In species with pigmented nerve cells, such as man and monkey, the accumulation may be much more pronounced because of the melanin affinity of MPTP and its metabolites. (author).

  18. Iron(II) complexes of new hexadentate 1,1,1-tris-(iminomethyl)ethane podands, and their 7-methyl-1,3,5-triazaadamantane rearrangement products.

    Science.gov (United States)

    Diener, Sara A; Santoro, Amedeo; Kilner, Colin A; Loughrey, Jonathan J; Halcrow, Malcolm A

    2012-04-07

    New iron(II) podand complexes have been prepared, by condensation of 2-(aminomethyl)-2-methyl-1,3-diaminopropane with 3 equiv of a heterocyclic aldehyde in the presence of hydrated Fe[BF(4)](2) or Fe[ClO(4)](2) as templates. The 2-(aminomethyl)-2-methyl-1,3-diaminopropane is prepared in situ by deprotonation of its trihydrochloride salt. The chloride must be removed from these reactions by precipitation with silver, to avoid the formation of the alternative 2,4,6-trisubstituted-7-methyl-1,3,5-triazaadamantane condensation products, or their FeCl(2) adducts. The crystal structures of two 2,4,6-tri(pyridyl)-7-methyl-1,3,5-triazaadamantane-containing species are presented, and contain two different geometric isomers of this tricyclic ring with three equatorial, or two equatorial and one axial, pyridyl substituents. Both structures feature strong C-HX (X = Cl or F) hydrogen bonding from the aminal C-H groups in the triazaadamantane ring. Five iron(II) podand complexes were successfully obtained, all of which contain low-spin iron centres.

  19. Selective bromination of 4-chloro-1-indanone and synthesis of (4-chloro-2, 3-dihydro-1H-indene-2-yl)methanamine

    OpenAIRE

    Jasouri, S.; Khalafy, J.; Badali, M.; Piltan, M.

    2010-01-01

    The synthesis of 4-chloro-1-indanone in four steps from 2-chlorobenzaldehyde was investigated. Bromination of this compound under various conditions occurred in the cyclopentanone ring, producing mono- and dibromo derivatives. Cyanation of 2-bromo-4-chloro-1-indanone followed by reduction gave (4-chloro-2, 3-dihydro-1H-indene-2-yl)methanamine in quantitative yield.

  20. Posttest analysis of a 1:4-scale prestressed concrete containment vessel model

    International Nuclear Information System (INIS)

    Dameron, R.A.; Rashid, Y.R.; Hessheimer, M.F.

    2003-01-01

    The Nuclear Power Engineering Corporation (NUPEC) of Japan and the U.S. Nuclear Regulatory Commission (NRC), Office of Nuclear Regulatory Research, co-sponsored a Cooperative Containment Research Program at Sandia National Laboratories (SNL) in Albuquerque, New Mexico. As part of the program, a prestressed concrete containment vessel (PCCV) model was subjected to a series of overpressurization tests at SNL beginning in July 2000 and culminating in a functional failure mode or Limit State Test (LST) in September 2000 and a Structural Failure Mode Test (SFMT) in November 2001. The PCCV model, uniformly scaled at 1:4, is representative of the containment structure of an actual Pressurized Water Reactor (PWR) plant (OHI-3) in Japan. The objectives of the pressurization tests were to obtain measurement of the structural response to pressure loading beyond design basis accident in order to validate analytical modeling, to find pressure capacity of the model, and to observe its failure mechanisms. This paper compares results of pretest analytical studies of the PCCV model to the PCCV high pressure test measurements and describes results of post-test analytical studies. These analyses have been performed by ANATECH Corp. under contract with Sandia National Laboratories. The post-test analysis represents the third phase of a comprehensive PCCV analysis effort. The first phase consisted of preliminary analyses to determine what finite element models would be necessary for the pretest prediction analyses, and the second phase consisted of the pretest prediction analyses. The principal objectives of the post-test analyses were: (1) to provide insights to improve the analytical methods for predicting the structural response and failure modes of a prestressed concrete containment, and (2) to evaluate by analysis any phenomena or failure mode observed during the test that had not been explicitly predicted by analysis. In addition to summarizing comparisons between measured

  1. Synthesis of New Pyrazolo[5,1-c]triazine, Triazolo[5,1-c]triazine, Triazino[4,3-b]indazole and Benzimidazo[2,1-c]triazine Derivatives Incorporating Chromen-2-one Moiety

    Energy Technology Data Exchange (ETDEWEB)

    Khalil, Mohamed A.; Sayed, Samia M.; Raslan, Mohamed A. [Aswan Univ., Aswan (Egypt)

    2013-10-15

    The versatile, hitherto unreported 3-(4-(2-phenyldiazenyl)-2-oxo-2H-chromen-3-yl)-3-oxopropanenitrile 3 was prepared by two convenient routes: either by the reaction of ethyl 4-(2-phenyldiazenyl)-2-oxo-2H-chromen-3-carboxylate 2 with acetonitrile in the presence of sodium hydride or by treatment of 4-(2-phenyldiazenyl)-3-(2-bromoacetyl)-2H-chromen-2-one 5 with potassium cyanide. Reaction of 3 with heterocyclic diazonium salts 6, 7, 14 and 17 furnished the corresponding hydrazones 8, 9, 15 and 18. The latter hydrazones underwent intramolecular cyclization into the corresponding pyrazolo[5,1-c]-1,2,4-triazine 10, 1,2,4-triazolo[5,1-c]-1,2,4-triazine 11, 1,2,4-triazino[4,3-b]indazole 16 and imidazo[2,1-c]-1,2,4-triazine 19 derivatives, respectively upon refluxing in pyridine.

  2. Synthesis, physical-chemical properties, antimicrobial and antifungal activity of some 2-(2-((5-(adamantane-1-yl-4-R-1,2,4-triazole-3-ylthioacetyl-N-R1–hydrazine-carbothioamides

    Directory of Open Access Journals (Sweden)

    V. M. Odyntsova

    2017-12-01

    Full Text Available Special attention of pharmaceutical scientists is attracted to the creation of new potential substances. They select natural heterocyclic molecules that exhibit various types of pharmacological activity as basic structures. Adamantane derivatives, as well as a number of other framework compounds, in the vast majority are biologically active substances. This fact causes interest to the given classes of organic compounds as potential sources for the development of new drugs. Due to the high pharmacological action of 1,2,4-triazole derivatives, the combination of adamantane and 1,2,4-triazole in one molecule can lead to the formation of high-level pharmacological substances. The aim of this work is the synthesis of some 2- (2 - ((5- (adamantane-1-yl -4-R-1,2,4-triasole-3-yl thio acetyl -N-R1-hydrazine-carbothioamides, study of their physical and chemical properties, antimicrobial and antifungal activity. Materials and methods. The chemical names of the compounds are given in accordance with the requirements of the IUPAC nomenclature (1979 and the recommendations of the IUPAC (1993. Study of the physical and chemical properties of 2-(2-((5-(adamantane-1-yl-4-R-1,2,4-triazole-3-ylthioacetyl-N-R1-hydrazine-carbothioamides have been carried out on the certified and licensed equipment in the ZSMU physical-chemical laboratories. The melting temperature was determined by an open capillary method on the Opti Melt MPA 100. The elemental composition of the synthesized compounds was determined on the universal analyzer Elementar Vario L cube (CHNS (standard – sulfanilamide. 1H NMR spectra were recorded on a spectrometer Varian Mercury VX-200 (1H, 200 MHz in dimethylsulfoxide-d6solvent (tetramethylsilane - internal standard and are decoded using ADVASP(tmAnalyzer program (Umatek International Inc.. Chromatographic mass spectral studies were performed on a gas-liquid chromatograph Agilent 1260 Infinity HPLC equipped with an Agilent 6120 mass spectrometer

  3. 2,4,6-Tri­amino-1,3,5-triazin-1-ium 3-(prop-2-eno­yloxy)propano­ate acrylic acid monosolvate monohydrate

    Science.gov (United States)

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

    2013-01-01

    The asymmetric unit of the title salt, C3H7N6 +·C6H7O4 −·C3H4O2·H2O, contains a 2,4,6-tri­amino-1,3,5-triazin-1-ium cation, a 3-(prop-2-eno­yloxy)propano­ate anion and acrylic acid and water solvent mol­ecules in a 1:1:1:1 ratio and with each species in a general position. In the crystal, the components are linked into a supra­molecular layer in the bc plane via a combination of O—H⋯O, N—H⋯N and N—H⋯O hydrogen bonding. The crystal studied was a non-merohedral twin, the minor component contribution being approximately 26%. PMID:23723892

  4. Poly[[[diaquacobalt(II]-bis[μ2-1,1′-(butane-1,4-diyldiimidazole-κ2N3:N3′

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available In the title compound, {[Co(C10H14N42(H2O2](NO32}n, the CoII ion lies on an inversion center and is six-coordinated in an octahedral environment by four N atoms from four different 1,1′-butane-1,4-diyldiimidazole ligands and two O atoms from the two water molecules. The CoII atoms are bridged by ligands, generating a two-dimensional (4,4-network. Adjacent fishnet planes are linked to the nitrate anions via O—H...O hydrogen bonds, forming a three-dimensional supramolecular structure.

  5. 2,3-Bis(2-chlorobenzylnaphthalene-1,4-dione

    Directory of Open Access Journals (Sweden)

    Seik Weng Ng

    2008-03-01

    Full Text Available The title disubstituted naphthalene-1,4-dione, C24H16Cl2O2, has the two chlorobenzyl substituents related by a non-crystallographic twofold rotation axis, generating a chiral conformation; both enantiomers are present. The two chlorobenzene rings are nearly perpendicular to the fused ring system, making angles of 88.8 (1 and 77.5 (1° with it.

  6. 3-Benzyl-4-ethyl-1H-1,2,4-triazole-5(4H)-thione.

    Science.gov (United States)

    Karczmarzyk, Zbigniew; Pitucha, Monika; Wysocki, Waldemar; Pachuta-Stec, Anna; Stańczuk, Andrzej

    2013-02-01

    The title compound, C(11)H(13)N(3)S, exists in the 5-thioxo tautomeric form. The benzene ring exhibits disorder with a refined ratio of 0.77 (2):0.23 (2) for components A and B with a common bridgehead C atom. The 1,2,4-triazole ring is essentially planar, with a maximum deviation of 0.002 (3) Å for the benzyl-substituted C atom, and forms dihedral angles of 88.94 (18) and 86.56 (49)° with the benzene rings of components A and B, respectively. The angle between the plane of the ethyl chain and the mean plane of 1,2,4-triazole ring is 88.55 (15)° and this conformation is stabilized by an intra-molecular C-H⋯S contact. In the crystal, pairs of N-H⋯S hydrogen bonds link mol-ecules into inversion dimers. π-π inter-actions are observed between the triazole and benzene rings, with centroid-centroid separations of 3.547 (4) and 3.544 (12) Å for components A and B, and slippages of 0.49 (6) and 0.58 (15) Å, respectively.

  7. 4-Aminobenzoic acid 4-methylpyridine/4-methylpyridinium 4-aminobenzoate 0.58/0.42: a redetermination from the original data

    Czech Academy of Sciences Publication Activity Database

    Fábry, Jan

    2017-01-01

    Roč. 73, Oct (2017), s. 1508-1512 ISSN 2056-9890 R&D Projects: GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : crystal structure * hydrogen bonding * symmetric hydrogen bonds * refinement constraints Subject RIV: CC - Organic Chemistry OBOR OECD: Organic chemistry

  8. Synthesis and Molecular Structure of 6-Amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one

    Directory of Open Access Journals (Sweden)

    Gene-Hsiang Lee

    2006-03-01

    Full Text Available The title compound 6-amino-3-benzylmercapto-1,2,4-triazolo[3,4-f][1,2,4]-triazin-8(7H-one (4, molecular formula C11H10N6OS, was obtained by the reaction of3-amino-2-benzyl-6-hydrazino-1,2,4-triazin-5(2H-one (3 with carbon disulfide in awater/pyridine mixture. Compound 4 can also be synthesized by reacting6-amino-3(2Hmercapto-1,2,4-triazolo[3,4-f][1,2,4]triazin-8(7H-one (7 with benzylbromide in methanolic ammonia water. The compound crystallizes in the monoclinicspace group P21/c with a = 7.2926(15, b = 14.456(2, c = 11.436(2 å, β = 105.30(2°, V= 1162.9(4 å3 and Z = 4, resulting in a density Dcalc of 1.567 g/cm3. Molecules of 4 arelinked by extensive intermolecular N-H···N and N-H···O hydrogen bonding [graph set R22 (9]. The structure is further stabilized by π-π stacking interactions. 2

  9. 21 CFR 178.3480 - Fatty alcohols, synthetic.

    Science.gov (United States)

    2010-04-01

    ... derived lauryl alcohol permitted as an intermediate in the synthesis of sodium lauryl sulfate used in..._locations.html. (1) Synthetic fatty alcohols. (i) Hexyl, octyl, decyl, lauryl, myristyl, cetyl, and stearyl... they may contain not more than 0.8 weight percent total diols. (ii) Lauryl, myristyl, cetyl, and...

  10. Synthesis and antimicrobial properties of 3-aryl-1-(1,1'-biphenyl-4-yl)-2-(1H-imidazol-1-yl)propanes as 'carba-analogues' of the N-arylmethyl-N-[(1,1'-biphenyl)-4-ylmethyl])-1H-imidazol-1-amines, a new class of antifungal agents.

    Science.gov (United States)

    Castellano, Sabrina; Stefancich, Giorgio; Chillotti, Annalisa; Poni, Graziella

    2003-08-01

    A new series of 3-phenyl-1-(1,1'-biphenyl-4-yl)-2-(1H-imidazol-1-yl)propane derivatives 2a-l (related to the antifungal bifonazole) was synthesized and tested for antimicrobial activity. A number of substituents on the phenyl ring were chosen to compare the relative biological properties with those of corresponding aza-analogues, previously described by us. The in vitro antifungal activities of the newly synthesized azoles were tested against several pathogenic fungi responsible for human disease. Test pathogens included representatives of yeasts (Candida albicans, Candida parapsilosis, Criptococcus neoformans), dermathophytes (Tricophyton verrucosum, Tricophyton rubrum, Microsporum gypseum) and moulds (Aspergillus fumigatus). Bifonazole and miconazole were used as reference drugs. Title compounds were prepared by alkylation of 1-biphenyl-4-yl-2-imidazol-1-yl-ethanone with the proper arylmethyl halide and subsequent reduction of corresponding ketones applying the Huang-Minlon modification of the Wolff-Kishner reaction.

  11. Polymers Containing 1, 3, 4-Oxadiazole Rings for Advanced Materials

    Directory of Open Access Journals (Sweden)

    Mariana-Dana Damaceanu

    2011-10-01

    Full Text Available This paper presents the synthesis, properties and potential applications of new polymers containing 1, 3, 4-oxadiazole rings, tacking into account the requirements of the modern technologies. Two classes of polymers containing oxadiazole rings were approached: polyamides and polyimides. All the polymers were characterized with respect to the identification of their chemical structure, solubility, molecular weights, film forming ability, thermal, dielectric and optical properties, and the behaviour of polyoxadiazole films upon irradiation with pulsed KrF laser. All the properties were discussed in correlation with their chemical structure and compared with those of related polymers.

  12. Evolution of Regions Containing Antibiotic Resistance Genes in FII-2-FIB-1 ColV-Colla Virulence Plasmids.

    Science.gov (United States)

    Moran, Robert A; Hall, Ruth M

    2018-05-01

    Three ColV virulence plasmids carrying antibiotic resistance genes were assembled from draft genome sequences of commensal ST95, ST131, and ST2705 Escherichia coli isolates from healthy Australians. Plasmids pCERC4, pCERC5, and pCERC9 include almost identical backbones containing FII-2 and FIB-1 replicons and the conserved ColV virulence region with an additional ColIa determinant. Only pCERC5 includes a complete, uninterrupted F-like transfer region and was able to conjugate. pCERC5 and pCERC9 contain Tn1721, carrying the tet(A) tetracycline resistance determinant in the same location, with Tn2 (bla TEM ; ampicillin resistance) interrupting the Tn1721 in pCERC5. pCERC4 has a Tn1721/Tn21 hybrid transposon carrying dfrA5 (trimethoprim resistance) and sul1 (sulfamethoxazole resistance) in a class 1 integron. Four FII-2:FIB-1 ColV-ColIa plasmids in the GenBank nucleotide database have a related transposon in the same position, but an IS26 has reshaped the resistance gene region, deleting 2,069 bp of the integron 3'-CS, including sul1, and serving as a target for IS26 translocatable units containing bla TEM , sul2 and strAB (streptomycin resistance), or aphA1 (kanamycin/neomycin resistance). Another ColV-ColIa plasmid containing a related resistance gene region has lost the FII replicon and acquired a unique transfer region via recombination within the resistance region and at oriT. Eighteen further complete ColV plasmid sequences in GenBank contained FIB-1, but the FII replicons were of three types, FII-24, FII-18, and a variant of FII-36.

  13. Assay of common sunscreen agents in suncare products by high-performance liquid chromatography on a cyanopropyl-bonded silica column.

    Science.gov (United States)

    Simeoni, Silvia; Tursilli, Rosanna; Bianchi, Anna; Scalia, Santo

    2005-06-15

    A rapid high-performance liquid chromatographic method was developed for the simultaneous assay of eight of the most common sunscreen agents (octyl-methoxycinnamate, oxybenzone, butyl-methoxydibenzoylmethane, octyl-salicilate, methylbenzylidene camphor, octyl-dimethylamminobenzoate, phenylbenzimidazole sulphonic acid and octocrylene) in sun protection products. Evaluation of the influence of different stationary phases and eluents on the separation selectivity showed that optimal resolution was obtained on a cyanopropyl-silica column eluted with methanol-acetonitrile-tetrahydrofuran-aqueous acetic acid. A small adjustment of the proposed chromatographic system (reduction in the aqueous content of the mobile phase) permitted also the determination of the extremely hydrophobic UV filter, methylene bis-benzotriazolyl tetramethylbutylphenol along with three other sunscreen agents, octyl-methoxycinnamate, oxybenzone, butyl-methoxydibenzoylmethane. Recoveries of the UV filters from the spiked formulation were between 95.7 and 103.7% and the precision of the method was better than 6.1% relative standard deviation. The developed HPLC procedure is suitable for quality control and photostability analyses of commercial suncare products.

  14. Synthesis and crystal structure of a homoleptic diruthenium complex containing tetra-2-pyridyl-1,4-pyrazine (tppz)

    Energy Technology Data Exchange (ETDEWEB)

    Graf, Marion; Mayer, Peter; Boettcher, Hans-Christian [Muenchen Univ. (Germany). Dept. Chemie

    2017-07-01

    Treatment of hydrated ruthenium(III) chloride with tetra-2-pyridyl-1,4-pyrazine (tppz) in refluxing ethoxyethanol afforded the homoleptic dinuclear complex [(tppz)Ru(μ-tppz)Ru(tppz)]{sup 4+} (1) besides small amounts of the species [Ru(tppz){sub 2}]{sup 2+}. The title complex 1 was obtained as purple crystals and characterized as its hexafluoridophosphate salt by NMR spectroscopy, mass spectrometry and microanalyses. The molecular structure of 1(PF{sub 6}){sub 4} has been established by X-ray crystallography.

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

    DEFF Research Database (Denmark)

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

    2006-01-01

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