4-Amino-3-mercapto-6-methyl-l,2,4-triazin-5(4H)-one 1 converted to 4-amino-6-methy-3-(methylthio)-1,2,4-triazin-5(4H)-one by methylation with methyl iodide.Controlled hydrazination of the resulting compound affo...4-Amino-3-mercapto-6-methyl-l,2,4-triazin-5(4H)-one 1 converted to 4-amino-6-methy-3-(methylthio)-1,2,4-triazin-5(4H)-one by methylation with methyl iodide.Controlled hydrazination of the resulting compound afforded 4-amino-3-hydrazinyl-6- methyl-l,2,4-triazin-5(4H)-one 2 as a building block,to the synthesis of some novel derivatives of[1,2,4]triazino- [4,3,b][1,2,4,5]tetrazepine 3-6,by the reaction with 3-chloropentane-2,4-dione,chloro acetonitrile,1,3-dichloroacetone,and methyl bromoacetate.This general synthetic procedure can be extended to the preparation of wide variety of tetrazepines using 1,2- bielectrophiles derivatives.展开更多
In situ attenuated total refletion-Fourier transform infrared spectroscopy(ATR-FTIR) was used to monitorand acquire spectral information on the synthesis of 4-amino-3,5-dimethyl pyrazole. Principal component analy-...In situ attenuated total refletion-Fourier transform infrared spectroscopy(ATR-FTIR) was used to monitorand acquire spectral information on the synthesis of 4-amino-3,5-dimethyl pyrazole. Principal component analy-sis(PCA) was used to determine the number of principle components(PCs). The score vectors of the PCs were ana-lysed using the simple-to-use interactive self-modelling mixture analysis(SIMPLISMA) algorithm to obtain spectraland concentration profiles for the reactants, intermediates and product. The vibrational frequencies of the interme-diates were calculated via density ftmctional theory(DFT) at the level of the B3LYP/6-31 l++G(d,p) basis set, and thegeometrical configurations of the intermediates were simultaneously optimized. Finally, a reasonable synthesismechanism for 4-amino-3,5-dimethyl pyrazole was determined based on the changes observed in the feature peaks.The results from the SIMPLISMA algorithm correlated well with the quantttm chemistry calculations. This provedthat the SIMPLISMA algorithm combined with ATR-FTIR can be used to detemfine the synthesis mechanism for4-amino-3,5-dimethyl pyrazole and can even provide a new, useful method to explore dynamic synthesis reactionmechanisms.展开更多
New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<s...New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).展开更多
New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<s...New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).展开更多
The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its...The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6)A, α = 112.566(1), β = 92.324(2), γ = 102.91(1)°, V= 1315.65(10) A^3, Z = 2, Dc = 1.344 g/cm^3,μ(MoKa) = 0.282 mm^-1, λ = 0.71073 A, F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C( 12)-H(12)…O(1) and C(28)-H(28)...O(1)# 1 hydrogen bonds were observed in the title compound.展开更多
The title compound (ethyl5-(4-(2-phenylacetamido)phenyl)-lH-pyrazole-3-carboxylate, C20H19N3O3) was synthesized by the reaction of Claisen condensation, cyclization, reduction and acylation. The structure was ch...The title compound (ethyl5-(4-(2-phenylacetamido)phenyl)-lH-pyrazole-3-carboxylate, C20H19N3O3) was synthesized by the reaction of Claisen condensation, cyclization, reduction and acylation. The structure was characterized by X-ray diffraction, MS, NMR and IR. It belongs to the monoclinic system, space group C2/c with a = 22.723(9), b = 9.324(4), c = 18.890(8) A, β = 114.259(6)°, V = 3649(3) A^3, Dc = 1.272 Mg·m^3, Z = 8, Mr = 349.38, p = 0.087 mm^-1, F(000) = 1472, the final R = 0.0615 and wR = 0.1643. The biological test shows that the title compound has a moderate acrosin inhibition activity.展开更多
Two new Schiff bases based on 5-chloro-3-methyl-1-phenyl-1 H-pyrazole-4-carbaldehyde, namely, N-((5-chloro-3-methyl-1-phenyl-1 H-pyrazol-4-yl)methylene)-4-morpholinoaniline(Ⅲa) and N-((5-chloro-3-methyl-1-phenyl-1 H-...Two new Schiff bases based on 5-chloro-3-methyl-1-phenyl-1 H-pyrazole-4-carbaldehyde, namely, N-((5-chloro-3-methyl-1-phenyl-1 H-pyrazol-4-yl)methylene)-4-morpholinoaniline(Ⅲa) and N-((5-chloro-3-methyl-1-phenyl-1 H-pyrazol-4-yl)methylene)-3-fluoro-4-morpholinoaniline(Ⅲb), were synthesized and characterized by IR, LC-MS, 1 H NMR and 13 C NMR spectroscopy. Meanwhile, the three-dimensional configurations of the two title compounds were further characterized by single-crystal X-ray diffraction analyses. Both the compounds are thermodynamically stable trans-isomers. Moreover, the fluorescence properties and antioxidant activities against DPPH of the two target compounds have been investigated, and the results showed that the title compounds both have fluorescence performance and certain antioxidant activities against DPPH radical.展开更多
An efficient triethylamine-catalyzed synthesis of 4-amino-3,5-dicyano-6-arylphthalates is described.A one-pot,simple pseudo four-component reaction between arylaldehydes,dialkyl acetylenedicarboxylates, and twice as m...An efficient triethylamine-catalyzed synthesis of 4-amino-3,5-dicyano-6-arylphthalates is described.A one-pot,simple pseudo four-component reaction between arylaldehydes,dialkyl acetylenedicarboxylates, and twice as much malononitrile gave 4-amino-3,5-dicyano-6-arylphthalates in good to excellent yields.展开更多
A series of six pyrazoles was synthesized by Michael-type addition reaction. The molecules 5-amino-1-aryl-1H-pyrazole-4-carbonitrile (3a-f) were synthesized from (ethoxymethylene)malo-nonitrile (1) and fluorinated and...A series of six pyrazoles was synthesized by Michael-type addition reaction. The molecules 5-amino-1-aryl-1H-pyrazole-4-carbonitrile (3a-f) were synthesized from (ethoxymethylene)malo-nonitrile (1) and fluorinated and non-fluorinated aryl hydrazines (2a-f) using ethanol and fluorinated ethanol as solvents at reflux. An excellent regio-selectivity was found when pyrazole derivatives were formed as an exclusive product. No other regioisomer or uncyclised hydrazide was observed. Their structures were confirmed by spectroscopy data (1H, 13C, 19F, COSY (correlation spectroscopy), HSQC (heteronuclear single-quantum correlation spectroscopy) and HMBC (heteronuclear multiple-bond correlation spectroscopy);MS (mass-spectrometry). The yields ranged from good to excellent (47% - 93%) under mild reaction conditions. It would indicate a high selectivity in the one-step work procedure. These products (3a-f) and derivatives have a potential academic and industrial use as key intermediates, in special, for application in crop protection.展开更多
The crystal of the title compound, 5-diazo-4-ethoxycarbonyl-3-methylthio pyrazole, has been prepared and determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 29.174(...The crystal of the title compound, 5-diazo-4-ethoxycarbonyl-3-methylthio pyrazole, has been prepared and determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 29.174(8), b = 4.7592(12), c = 15.956(4) ? b = 117.632(4), C7H8N4O2S, Mr = 212.23, V = 1962.7(9) ?, Z = 8, Dx = 1.436 g/cm3, S = 1.000, m(MoKa) = 0.31 mm-1, T = 298(2) K, F(000) = 880, R = 0.0658 and wR = 0.1741 for 1091 independent reflections with I ≥ 2s(I). The crystal of the title compound is formed with p-p interactions through electrostatic attractions. Moreover, no HSO4- exists in the crystal structure. Therefore, only diazo pyrazole was obtained rather than either diazonium salt of the corresponding pyrazole or diazoaminopyrazole when 5-amino-4-ethoxycarbonyl-3-methylthio pyrazole was diazotized with sodium nitrite, catalyzed by sulfuric acid at 0 ℃.展开更多
Two new alkaline earth metal coordination polymers constructed from the deriva-tive of 1,2,4-triazole are presented herein,namely,{[Sr(AmTAZAc)2(H2O)]}(1) and {[Ba(AmTAZAc)2(H2O)]}(2)(AmTAZAc = 3-amino-1H...Two new alkaline earth metal coordination polymers constructed from the deriva-tive of 1,2,4-triazole are presented herein,namely,{[Sr(AmTAZAc)2(H2O)]}(1) and {[Ba(AmTAZAc)2(H2O)]}(2)(AmTAZAc = 3-amino-1H-1,2,4-triazole-5-carboxylate),which have been synthesized by using the layering method and structurally characterized by elemental analysis,IR,and single-crystal X-ray diffraction.Complexes 1 and 2 are isostructural,and both crystallize in the orthorhombic system,space group Fdd2.X-ray structural analysis shows that 1 or 2 has an intriguing 3-D infinite network of(318.438.510) topology based on a 2-D sheet structure of(4,4) net.The result shows that noncovalent interactions play an important role in strengthening the whole structures of the compounds.展开更多
Persistent postsurgical pain is a serious issue in public health, which has received increased interest in recent years. Previous studies have reported that psychological factors promote the development of chronic pos...Persistent postsurgical pain is a serious issue in public health, which has received increased interest in recent years. Previous studies have reported that psychological factors promote the development of chronic postsurgical pain. However, it is unclear how chronification of postsurgical pain occurs. The α-amino-3-hydroxy-5-methyl-4-isoxazole-propionic acid receptor(AMPA) phosphorylation in the central nervous system plays a critical role in synaptic plasticity and contributes to central sensitization and chronic pain development. Here, we discuss the role of AMPA receptor regulation in stress-induced pain chronification after surgery.展开更多
Two aromatic multicarboxylate ligands tuned Zn(Ⅱ) coordination polymers, namely, {[Zn0.5(H2L)(tp)0.5(H2O)]H2O}n(1) and {[Zn2(HL)(btc)(H2O)]H2O}n(2)(H2L = 3-(1 Hpyrazol-4-yl)-5-(pyridin-3-yl)-1,2,4-triazole, H2tp = te...Two aromatic multicarboxylate ligands tuned Zn(Ⅱ) coordination polymers, namely, {[Zn0.5(H2L)(tp)0.5(H2O)]H2O}n(1) and {[Zn2(HL)(btc)(H2O)]H2O}n(2)(H2L = 3-(1 Hpyrazol-4-yl)-5-(pyridin-3-yl)-1,2,4-triazole, H2tp = terephthalic acid;H3 btc = 1,3,5-benzenetricarboxylic) have been synthesized. Their structures were characterized by single-crystal X-ray diffraction analysis, elemental analyses and infrared spectra. Compound 1 possesses a one-dimensional chain structure and is finally extended into a three-dimensional supramolecular architecture though hydrogen bonding interactions. Compound 2 shows a three-dimensional framework. Meanwhile, compounds 1 and 2 exhibit luminescent emission in the solid, and can be investigated as potential luminescent materials.展开更多
The reaction mechanism of 2-methoxybenzaldehyde, 4-bromo-indanone, malononitrile and ammonium acetate one-pot to form 6-(2-methoxyphenyl)-2-amino-6-bromo-5 Hindeno[1,2-b]pyridine-3-carbonitrile was studied by densit...The reaction mechanism of 2-methoxybenzaldehyde, 4-bromo-indanone, malononitrile and ammonium acetate one-pot to form 6-(2-methoxyphenyl)-2-amino-6-bromo-5 Hindeno[1,2-b]pyridine-3-carbonitrile was studied by density functional theory. The geometries of the reactants, transition states, intermediates and products were optimized at the PW91/DNP level. Vibration analysis was carried out to confirm the transition state structure. Reaction pathways were investigated in this study. The result indicates that the reaction Re→ TSB1→IMB1→ TSB2→ IMB2→TSB3→IMB3→TSB4→IMB4→TSB5→IMB5→TSB6→IMB6→TSB7→IMB7→ TSB8→IMB8→TSB9→IMB9→P2 is the main pathway, the activation energy of which is the lowest. The dominant product predicted theoretically is in agreement with the experiment results.展开更多
Compound 5-methyl-2-phenyl-4-[(Z)-3-tolylamino-phenylmethylene]pyrazol-3(2H)-one (C24H21N3O) crystallizes in the triclinic system, space group P1, with a = 9.267(3), b = 9.904(4),c = 12.035(4) A°, α ...Compound 5-methyl-2-phenyl-4-[(Z)-3-tolylamino-phenylmethylene]pyrazol-3(2H)-one (C24H21N3O) crystallizes in the triclinic system, space group P1, with a = 9.267(3), b = 9.904(4),c = 12.035(4) A°, α = 97.896(6), β = 103.865(6), γ = 107.950(6)°, Mr= 367.44, Z = 2, V = 993.2(6)A°^3,Dc = 1.229 g/cm^3,μ(MoKa) = 0.077 mm^-1 and F(000) = 388. The structure was refined to R =0.0444 and wR = 0.1199 for 2903 observed reflections (I 〉 2σ(I)). The results of ^1H NMR and single-crystal X-ray diffraction studies showed the enamine character of the compound. The strong intramolecular hydrogen bonds in the large conjugate system, together with weak intermolecular C-H……π hydrogen bonding and π……π stacking, lead to the formation of a multi-dimensional supramolecular network.展开更多
The BMPPT (4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-thione)was synthesized from BMPP. Its m.p. is 106-108℃. The results of the element analysis are as follows: C, 68.51%, H, 4.51%, N, 9.26%, S, 11.47%, wh...The BMPPT (4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-thione)was synthesized from BMPP. Its m.p. is 106-108℃. The results of the element analysis are as follows: C, 68.51%, H, 4.51%, N, 9.26%, S, 11.47%, which are in conformity with the theoretical value (C, 69.15%, H, 4.76%, N, 9.52%, S, 10.90%). The solvent extraction of Th4+ from nitric acid solution by BMPPT in benzene was studied. The extraction ability of BMPPT is not so high as that of its parent (BMPP). The Th4+ distribution ratio (DTh) increases with the increasing pH of the aqueous phase, and pH1/2 for Th4+ was 3.2 ([BMPPT]=0.10 mol/L). When the pH increases, the distribution ratio of Th4+ increases linearly with the slope of 1 .59. When the concentration of BMPPT increases, the distribution ratio of Th4+ increases rapidly. The lgDTh-lg[BMPPT] is linear with the slope of 1.42 and the extraction mechanism is the cation ion-exchange.展开更多
文摘4-Amino-3-mercapto-6-methyl-l,2,4-triazin-5(4H)-one 1 converted to 4-amino-6-methy-3-(methylthio)-1,2,4-triazin-5(4H)-one by methylation with methyl iodide.Controlled hydrazination of the resulting compound afforded 4-amino-3-hydrazinyl-6- methyl-l,2,4-triazin-5(4H)-one 2 as a building block,to the synthesis of some novel derivatives of[1,2,4]triazino- [4,3,b][1,2,4,5]tetrazepine 3-6,by the reaction with 3-chloropentane-2,4-dione,chloro acetonitrile,1,3-dichloroacetone,and methyl bromoacetate.This general synthetic procedure can be extended to the preparation of wide variety of tetrazepines using 1,2- bielectrophiles derivatives.
文摘In situ attenuated total refletion-Fourier transform infrared spectroscopy(ATR-FTIR) was used to monitorand acquire spectral information on the synthesis of 4-amino-3,5-dimethyl pyrazole. Principal component analy-sis(PCA) was used to determine the number of principle components(PCs). The score vectors of the PCs were ana-lysed using the simple-to-use interactive self-modelling mixture analysis(SIMPLISMA) algorithm to obtain spectraland concentration profiles for the reactants, intermediates and product. The vibrational frequencies of the interme-diates were calculated via density ftmctional theory(DFT) at the level of the B3LYP/6-31 l++G(d,p) basis set, and thegeometrical configurations of the intermediates were simultaneously optimized. Finally, a reasonable synthesismechanism for 4-amino-3,5-dimethyl pyrazole was determined based on the changes observed in the feature peaks.The results from the SIMPLISMA algorithm correlated well with the quantttm chemistry calculations. This provedthat the SIMPLISMA algorithm combined with ATR-FTIR can be used to detemfine the synthesis mechanism for4-amino-3,5-dimethyl pyrazole and can even provide a new, useful method to explore dynamic synthesis reactionmechanisms.
文摘New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).
文摘New cobalt(II) complex, [Co(O<sub>2</sub>C<sub>15</sub>H<sub>11</sub>N<sub>2</sub>S)<sub>2</sub>(OH<sub>2</sub>)<sub>2</sub>]∙2H<sub>2</sub>O (1∙2H<sub>2</sub>O), has been synthesized upon reaction of cobalt chloride hexahydrate (Co(Cl)<sub>2</sub>∙6H<sub>2</sub>O) with 3-methyl-1-Phenyl-4-(2-thienoyl)-pyrazol-5-one (referred as HL) in ethanol at room temperature. Single crystal X-ray diffraction (XRD), spectroscopic methods, and microelemental analyses were used to characterize 1∙2H<sub>2</sub>O. Compound 1∙2H<sub>2</sub>O crystallizes in the orthorhombic crystal system with a Pbca space group and with the cobalt atom being pseudo-octahedral coordinated. The broth microdilution technique was used to screen the free ligand (HL) and the complex (1∙2H<sub>2</sub>O) for antimicrobial activities. HL has a low activity (MIC > 100 μg/mL) on all microorganisms, whereas compound 1∙2H<sub>2</sub>O displayed moderate activity (10 ∙2H<sub>2</sub>O exhibited bactericidal and fungicidal activity respectively on all the bacteria and yeasts tested. These findings reveal that the antimicrobial activity of HL was enhanced upon coordination to Co(II) ion against all microorganisms (bacteria and fungus).
基金the Science Research Foundation of Henan Institute of Science and Technology (No. 06036)
文摘The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6)A, α = 112.566(1), β = 92.324(2), γ = 102.91(1)°, V= 1315.65(10) A^3, Z = 2, Dc = 1.344 g/cm^3,μ(MoKa) = 0.282 mm^-1, λ = 0.71073 A, F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C( 12)-H(12)…O(1) and C(28)-H(28)...O(1)# 1 hydrogen bonds were observed in the title compound.
基金supported by the Science and technology support program of Jiangsu Province (2010, BE2010682)
文摘The title compound (ethyl5-(4-(2-phenylacetamido)phenyl)-lH-pyrazole-3-carboxylate, C20H19N3O3) was synthesized by the reaction of Claisen condensation, cyclization, reduction and acylation. The structure was characterized by X-ray diffraction, MS, NMR and IR. It belongs to the monoclinic system, space group C2/c with a = 22.723(9), b = 9.324(4), c = 18.890(8) A, β = 114.259(6)°, V = 3649(3) A^3, Dc = 1.272 Mg·m^3, Z = 8, Mr = 349.38, p = 0.087 mm^-1, F(000) = 1472, the final R = 0.0615 and wR = 0.1643. The biological test shows that the title compound has a moderate acrosin inhibition activity.
基金supported by the Jiangsu Province College Students’ Practice and Innovation Training Program(No.201810323007Z)
文摘Two new Schiff bases based on 5-chloro-3-methyl-1-phenyl-1 H-pyrazole-4-carbaldehyde, namely, N-((5-chloro-3-methyl-1-phenyl-1 H-pyrazol-4-yl)methylene)-4-morpholinoaniline(Ⅲa) and N-((5-chloro-3-methyl-1-phenyl-1 H-pyrazol-4-yl)methylene)-3-fluoro-4-morpholinoaniline(Ⅲb), were synthesized and characterized by IR, LC-MS, 1 H NMR and 13 C NMR spectroscopy. Meanwhile, the three-dimensional configurations of the two title compounds were further characterized by single-crystal X-ray diffraction analyses. Both the compounds are thermodynamically stable trans-isomers. Moreover, the fluorescence properties and antioxidant activities against DPPH of the two target compounds have been investigated, and the results showed that the title compounds both have fluorescence performance and certain antioxidant activities against DPPH radical.
基金the financial support from the Research Council of Payame Noor University(PNU),Abhar-lran, and my colleague Ismail Hasani Asl
文摘An efficient triethylamine-catalyzed synthesis of 4-amino-3,5-dicyano-6-arylphthalates is described.A one-pot,simple pseudo four-component reaction between arylaldehydes,dialkyl acetylenedicarboxylates, and twice as much malononitrile gave 4-amino-3,5-dicyano-6-arylphthalates in good to excellent yields.
文摘A series of six pyrazoles was synthesized by Michael-type addition reaction. The molecules 5-amino-1-aryl-1H-pyrazole-4-carbonitrile (3a-f) were synthesized from (ethoxymethylene)malo-nonitrile (1) and fluorinated and non-fluorinated aryl hydrazines (2a-f) using ethanol and fluorinated ethanol as solvents at reflux. An excellent regio-selectivity was found when pyrazole derivatives were formed as an exclusive product. No other regioisomer or uncyclised hydrazide was observed. Their structures were confirmed by spectroscopy data (1H, 13C, 19F, COSY (correlation spectroscopy), HSQC (heteronuclear single-quantum correlation spectroscopy) and HMBC (heteronuclear multiple-bond correlation spectroscopy);MS (mass-spectrometry). The yields ranged from good to excellent (47% - 93%) under mild reaction conditions. It would indicate a high selectivity in the one-step work procedure. These products (3a-f) and derivatives have a potential academic and industrial use as key intermediates, in special, for application in crop protection.
基金Project supported by the National Natural Science Foundation of China (No. 20172031) the Research Fund for the Doctoral Program of High Education,China
文摘The crystal of the title compound, 5-diazo-4-ethoxycarbonyl-3-methylthio pyrazole, has been prepared and determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 29.174(8), b = 4.7592(12), c = 15.956(4) ? b = 117.632(4), C7H8N4O2S, Mr = 212.23, V = 1962.7(9) ?, Z = 8, Dx = 1.436 g/cm3, S = 1.000, m(MoKa) = 0.31 mm-1, T = 298(2) K, F(000) = 880, R = 0.0658 and wR = 0.1741 for 1091 independent reflections with I ≥ 2s(I). The crystal of the title compound is formed with p-p interactions through electrostatic attractions. Moreover, no HSO4- exists in the crystal structure. Therefore, only diazo pyrazole was obtained rather than either diazonium salt of the corresponding pyrazole or diazoaminopyrazole when 5-amino-4-ethoxycarbonyl-3-methylthio pyrazole was diazotized with sodium nitrite, catalyzed by sulfuric acid at 0 ℃.
基金Supported by the National Natural Science Foundation of China (Nos. 20771006 and 20901004)
文摘Two new alkaline earth metal coordination polymers constructed from the deriva-tive of 1,2,4-triazole are presented herein,namely,{[Sr(AmTAZAc)2(H2O)]}(1) and {[Ba(AmTAZAc)2(H2O)]}(2)(AmTAZAc = 3-amino-1H-1,2,4-triazole-5-carboxylate),which have been synthesized by using the layering method and structurally characterized by elemental analysis,IR,and single-crystal X-ray diffraction.Complexes 1 and 2 are isostructural,and both crystallize in the orthorhombic system,space group Fdd2.X-ray structural analysis shows that 1 or 2 has an intriguing 3-D infinite network of(318.438.510) topology based on a 2-D sheet structure of(4,4) net.The result shows that noncovalent interactions play an important role in strengthening the whole structures of the compounds.
基金Supported by The National Institute of Dental and Craniofacial Research Grants,Nos.R01 DE022880 and K02 DE023551
文摘Persistent postsurgical pain is a serious issue in public health, which has received increased interest in recent years. Previous studies have reported that psychological factors promote the development of chronic postsurgical pain. However, it is unclear how chronification of postsurgical pain occurs. The α-amino-3-hydroxy-5-methyl-4-isoxazole-propionic acid receptor(AMPA) phosphorylation in the central nervous system plays a critical role in synaptic plasticity and contributes to central sensitization and chronic pain development. Here, we discuss the role of AMPA receptor regulation in stress-induced pain chronification after surgery.
基金financially supported by the National Natural Science Foundation of China(21571093)
文摘Two aromatic multicarboxylate ligands tuned Zn(Ⅱ) coordination polymers, namely, {[Zn0.5(H2L)(tp)0.5(H2O)]H2O}n(1) and {[Zn2(HL)(btc)(H2O)]H2O}n(2)(H2L = 3-(1 Hpyrazol-4-yl)-5-(pyridin-3-yl)-1,2,4-triazole, H2tp = terephthalic acid;H3 btc = 1,3,5-benzenetricarboxylic) have been synthesized. Their structures were characterized by single-crystal X-ray diffraction analysis, elemental analyses and infrared spectra. Compound 1 possesses a one-dimensional chain structure and is finally extended into a three-dimensional supramolecular architecture though hydrogen bonding interactions. Compound 2 shows a three-dimensional framework. Meanwhile, compounds 1 and 2 exhibit luminescent emission in the solid, and can be investigated as potential luminescent materials.
基金Project supported by the Scientific and Technological Research Program of Chongqing Municipal Education Commission(KJ1601215,KJ15012002)the Ministry of Education “Chunhui Plan”(Z2016177)
文摘The reaction mechanism of 2-methoxybenzaldehyde, 4-bromo-indanone, malononitrile and ammonium acetate one-pot to form 6-(2-methoxyphenyl)-2-amino-6-bromo-5 Hindeno[1,2-b]pyridine-3-carbonitrile was studied by density functional theory. The geometries of the reactants, transition states, intermediates and products were optimized at the PW91/DNP level. Vibration analysis was carried out to confirm the transition state structure. Reaction pathways were investigated in this study. The result indicates that the reaction Re→ TSB1→IMB1→ TSB2→ IMB2→TSB3→IMB3→TSB4→IMB4→TSB5→IMB5→TSB6→IMB6→TSB7→IMB7→ TSB8→IMB8→TSB9→IMB9→P2 is the main pathway, the activation energy of which is the lowest. The dominant product predicted theoretically is in agreement with the experiment results.
文摘Compound 5-methyl-2-phenyl-4-[(Z)-3-tolylamino-phenylmethylene]pyrazol-3(2H)-one (C24H21N3O) crystallizes in the triclinic system, space group P1, with a = 9.267(3), b = 9.904(4),c = 12.035(4) A°, α = 97.896(6), β = 103.865(6), γ = 107.950(6)°, Mr= 367.44, Z = 2, V = 993.2(6)A°^3,Dc = 1.229 g/cm^3,μ(MoKa) = 0.077 mm^-1 and F(000) = 388. The structure was refined to R =0.0444 and wR = 0.1199 for 2903 observed reflections (I 〉 2σ(I)). The results of ^1H NMR and single-crystal X-ray diffraction studies showed the enamine character of the compound. The strong intramolecular hydrogen bonds in the large conjugate system, together with weak intermolecular C-H……π hydrogen bonding and π……π stacking, lead to the formation of a multi-dimensional supramolecular network.
文摘The BMPPT (4-benzoyl-2,4-dihydro-5-methyl-2-phenyl-3H-pyrazol-3-thione)was synthesized from BMPP. Its m.p. is 106-108℃. The results of the element analysis are as follows: C, 68.51%, H, 4.51%, N, 9.26%, S, 11.47%, which are in conformity with the theoretical value (C, 69.15%, H, 4.76%, N, 9.52%, S, 10.90%). The solvent extraction of Th4+ from nitric acid solution by BMPPT in benzene was studied. The extraction ability of BMPPT is not so high as that of its parent (BMPP). The Th4+ distribution ratio (DTh) increases with the increasing pH of the aqueous phase, and pH1/2 for Th4+ was 3.2 ([BMPPT]=0.10 mol/L). When the pH increases, the distribution ratio of Th4+ increases linearly with the slope of 1 .59. When the concentration of BMPPT increases, the distribution ratio of Th4+ increases rapidly. The lgDTh-lg[BMPPT] is linear with the slope of 1.42 and the extraction mechanism is the cation ion-exchange.