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
An efficient,economical,and phosgene-free approach was developed for the preparation of l,4-dihydro-2H-3,l-benzoxazin-2-one from 2-aminobenzyl alcohol.In terms of its key features,this reaction uses the cheap and recy...An efficient,economical,and phosgene-free approach was developed for the preparation of l,4-dihydro-2H-3,l-benzoxazin-2-one from 2-aminobenzyl alcohol.In terms of its key features,this reaction uses the cheap and recyclable non-metal selenium as a catalyst instead of the noble metal palladium;carbon monoxide as a carbonylation agent instead of virulent phosgene or one of its derivatives;and oxygen as an oxidant.The selenium-catalyzed oxidative carbonylation reaction of2-aminobenzyl alcohol proceeded efficiently in a single pot in the presence of triethylamine to afford l,4-dihydro-2H-3,l-benzoxazin-2-one in 87%yield.Furthermore,the selenium catalyst was readily recovered and recycled,affording a product yield of 80%after five cycles.展开更多
The relationships between 17α,20β dihydroxy 4 pregnene 3 one (17α,20β DP) and plasma IgM and total protein levels were investigated in rainbow trout, Oncorhynchus mykiss .IgM and total protein levels decre...The relationships between 17α,20β dihydroxy 4 pregnene 3 one (17α,20β DP) and plasma IgM and total protein levels were investigated in rainbow trout, Oncorhynchus mykiss .IgM and total protein levels decreased in both sexes of mature rainbow trout when 17α,20β DP levels increased during the spawning season,while the elevated 17α,20β DP suppressed IgM levels and reversibly enhanced total protein concentrations in immature trout.This represents the first report of the effect of 17α,20β DP on fish immunity.These data suggest that the increase of 17α,20β DP in spawning season may be related to infectious skin diseases.展开更多
Heteropoly acids efficiently catalyzed the cyclocondensation reaction of anthranilamide with aldehydes in water at ambient temperature and afforded the corresponding 2,3-dihydro-4(1H)-quinazolinones compounds in goo...Heteropoly acids efficiently catalyzed the cyclocondensation reaction of anthranilamide with aldehydes in water at ambient temperature and afforded the corresponding 2,3-dihydro-4(1H)-quinazolinones compounds in good to excellent yields.This method provides mild reaction conditions and clean reaction profiles,using a small quantity of catalyst and a simple workup procedure.展开更多
The 3?Nitro?1,2,4?triazole?5?one(NTO)is a high energy density materials of keen interest for both commercial and scientific worlds owing to its reduced sensitivity,better thermal stability and high performances. It pl...The 3?Nitro?1,2,4?triazole?5?one(NTO)is a high energy density materials of keen interest for both commercial and scientific worlds owing to its reduced sensitivity,better thermal stability and high performances. It plays a significant role to replace the current energetic ingredients. In this review,we summarize various strategies involved in the synthesis of NTO as well as the existing approaches to tailor its particle morphology and sizes. The most prominent properties of NTO,such as insensitivity and performance,which are usually required to produce efficient formulations,have been concisely discussed. In addition,this overview reports on some newer forms of NTO including derivatives and co?crystals available in the literature,which can enhance the NTO features and extend its applications. The advantages and shortcomings of various NTO forms for specific and potential use are also highlighted together with the attempts made to overcome these issues. Therefore,efforts will certainly continue to improve characteristics and performances of NTO either by chemical modification or by co?crystallization in order to produce promising formulations for widespread applications in the near future.展开更多
Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3...Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.展开更多
The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4(3H)-one (C16H18N2O3, Mr = 286.32) has been prepared and determined by singlecrystal X-ray diffraction. The crystal is ...The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4(3H)-one (C16H18N2O3, Mr = 286.32) has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167(14), b = 13.113(1), c = 8.378(1) A, β = 98.992(2)^o, V = 1488.4(3) A^3, Z = 4, Dc = 1.278, F(000) = 608, μ = 0.089 mm^-1, MoKa radiation (2 = 0.71073), R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.展开更多
2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl ...2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl chloride catalysts the reaction is limited to give only 1,8-dioxo-octahydroxanthenes 3a-k in very good yields.展开更多
A new one-pot neat synthesis of some 5-aryl-2,4-dihydro-3H- 1,2,4-triazol-3-ones through cyclocondensation of ethyl carbazate with aryl nitriles catalyzed by DMAP as an efficient and basic nucleophilic catalyst is des...A new one-pot neat synthesis of some 5-aryl-2,4-dihydro-3H- 1,2,4-triazol-3-ones through cyclocondensation of ethyl carbazate with aryl nitriles catalyzed by DMAP as an efficient and basic nucleophilic catalyst is described.展开更多
The synthesis of 3-(2'-hydroxybutyl)isobenzofuran-1(3H)-onel from phthalicanhydride via the intermediate 3-(2'-oxoethyl) isobenzofuran-1(3H)-one 6 was described.
Solvent extraction of palladium (Ⅱ) from hydrochloric acid solution with 2-n-octyl-4-isothiazolin-3-one (OIT)/cyclohexane was studied. Effects of different parameters on extraction efficiency were evaluated. 99.9...Solvent extraction of palladium (Ⅱ) from hydrochloric acid solution with 2-n-octyl-4-isothiazolin-3-one (OIT)/cyclohexane was studied. Effects of different parameters on extraction efficiency were evaluated. 99.96 % and 98.26 % palladium (Ⅱ) could be effectively extracted with 0.018 mol·L^-1 OIT/cyclohexane of 0.1 and 4.0 mol·L^-1 HCl medium, respectively. Nonpolar solvent and low acidity could improve the extracting efficiency, and successfully strip palladium (Ⅱ) from the loaded organic phase was achieved with 0.5 mol·L^-1 (NH2)2CS solution. It was proposed that the extraction of Pd com-plexes from HCl medium proceeded through the ion-association mechanism by slope method, NMR and FF-IR spectra.展开更多
The single crystal of the title compound (C12H8N2O2, Mr = 212.20) has been obtained by oxidation of 2-aminophenol in methanol solution with irradiation of sunlight. The crystal belongs to monoclinic space group P21/c ...The single crystal of the title compound (C12H8N2O2, Mr = 212.20) has been obtained by oxidation of 2-aminophenol in methanol solution with irradiation of sunlight. The crystal belongs to monoclinic space group P21/c with cell dimensions of a = 12.925(2), b = 5.077(3), c = 14.768(3)? b = 99.38(1), V = 956.2(5)?, Z = 4, Dc = 1.474 g/cm3, = 0.103 mm-1, R = 0.054, wR = 0.074 for 785 observed reflections (I > 2s(I)). The molecule consists of three coplanar rings. Much different CC distances (1.494(4)?and 1.343(6) ? observed within the quinoidal ring show the pattern of bond fixation expected for the Kekule formula.展开更多
Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as ...Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as the catalysts for the synthesis of bisdihydropyrimidin -2(1H)-ones from aromatic dialdehydes,1,3-dicarbonyl compounds and urea at 90℃under solvent-free conditions.展开更多
The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expect...The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632(1), b = 7.816(1), c = 28.082(5) A,β = 96.18(1)°, V= 1665.48(51) A^3, Z= 4, Dc = 1.341 g/cm^3, F(000) = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C(11)-C(16) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0.03 A) with the dihedral angle between them of 9.8%.展开更多
The title compound 3-(2,4-dichlorophenyl)-4-dydroxy-3-(2,4-dichlorophenyl)-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-(2,4-dichlorophenyl-acetyl)-1-hydr...The title compound 3-(2,4-dichlorophenyl)-4-dydroxy-3-(2,4-dichlorophenyl)-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-(2,4-dichlorophenyl-acetyl)-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192(3), b = 10.5053(5), c = 10.5811(5)A,α = 71.681(10), β = 78.905(12), γ = 81.036(12)°, C15H14C1203, Mr = 313.18, V= 702.44(6)A3, Z = 2, De= 1.481 g/cm^3, F(000) = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ(I) and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O(1)-H(101)…O(2).展开更多
Alkylamino-5, 6, 7, 8-tetrahydrobenzothieno [2, 3-d] pyrimidin-4(3H)-ones 7 weresynthesized by a new selective synthetic method, which includes aza-Wittig reaction of imino-phosphorane 4 with aromatic isocynate to giv...Alkylamino-5, 6, 7, 8-tetrahydrobenzothieno [2, 3-d] pyrimidin-4(3H)-ones 7 weresynthesized by a new selective synthetic method, which includes aza-Wittig reaction of imino-phosphorane 4 with aromatic isocynate to give carbodiimide 5 and subsequent reaction of 5 withvarious aliphatic primary amine in the presence of EtO-Na+.展开更多
Twelve Mannich base derivatives of 1,2-benzisothiazolin-3-one were synthesized by the reaction of 1,2-benzisothiazol-3(2H)-one (BIT) with different amines and formaldehyde. All the compounds were characterized by ...Twelve Mannich base derivatives of 1,2-benzisothiazolin-3-one were synthesized by the reaction of 1,2-benzisothiazol-3(2H)-one (BIT) with different amines and formaldehyde. All the compounds were characterized by elemental analysis, IR spectroscopy, MS and 1H NMR. The crystal structure for 2,2'-methylenebis(benzo[d]isothiazol-3(2H)-one) (3) has been determined by X-ray single-crystal structure analysis. Compound 3 (C15HIoN202S2) crystallizes in the monoclinic system, space group C2/c with a = 25.052(8), b = 4.510(1), c = 11.948(4) A, β = 100.992(4)°, V= 1325.2(7) A3, Mr = 314.37, Dc = 1.576 Mg.m-3, p = 0.25 mm-1, F(000) = 648, Z = 4, R = 0.034 and wR = 0.087. The preliminary biological test indicated that the compounds (2b, 2c) showed growth inhibitory activity against the gram-positive and gram-negative bacteria.展开更多
The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ra...The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of orthorhombic,space group Pccn with a = 16.7246(10),b = 19.6626(12),c = 9.3013(6) ,V = 3058.7(3) 3,Z = 8,Dc = 1.402 g/cm3,μ = 0.269 mm-1,F(000) = 1344,the final R = 0.0506 and wR = 0.1464 for 2568 reflections with I 〉 2σ(I).In addition,disordered C(14) and C(15) atoms exist in the crystal structure.展开更多
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supported by the Program for Changjiang Scholars and Innovative Research Team in University(IRT1061)the Program for Innovative Research Team in Science and Technology in University of Henan Province(15IRTSTHN003)+1 种基金the Young Backbone Teachers Training Fund of the Education Department of Henan Province(2013GGJS-059)Henan Normal University(2011-8)
文摘An efficient,economical,and phosgene-free approach was developed for the preparation of l,4-dihydro-2H-3,l-benzoxazin-2-one from 2-aminobenzyl alcohol.In terms of its key features,this reaction uses the cheap and recyclable non-metal selenium as a catalyst instead of the noble metal palladium;carbon monoxide as a carbonylation agent instead of virulent phosgene or one of its derivatives;and oxygen as an oxidant.The selenium-catalyzed oxidative carbonylation reaction of2-aminobenzyl alcohol proceeded efficiently in a single pot in the presence of triethylamine to afford l,4-dihydro-2H-3,l-benzoxazin-2-one in 87%yield.Furthermore,the selenium catalyst was readily recovered and recycled,affording a product yield of 80%after five cycles.
文摘The relationships between 17α,20β dihydroxy 4 pregnene 3 one (17α,20β DP) and plasma IgM and total protein levels were investigated in rainbow trout, Oncorhynchus mykiss .IgM and total protein levels decreased in both sexes of mature rainbow trout when 17α,20β DP levels increased during the spawning season,while the elevated 17α,20β DP suppressed IgM levels and reversibly enhanced total protein concentrations in immature trout.This represents the first report of the effect of 17α,20β DP on fish immunity.These data suggest that the increase of 17α,20β DP in spawning season may be related to infectious skin diseases.
基金the financial support of Key Laboratory of Resources and Environment Chemistry of West China(No.XZ0704).
文摘Heteropoly acids efficiently catalyzed the cyclocondensation reaction of anthranilamide with aldehydes in water at ambient temperature and afforded the corresponding 2,3-dihydro-4(1H)-quinazolinones compounds in good to excellent yields.This method provides mild reaction conditions and clean reaction profiles,using a small quantity of catalyst and a simple workup procedure.
文摘The 3?Nitro?1,2,4?triazole?5?one(NTO)is a high energy density materials of keen interest for both commercial and scientific worlds owing to its reduced sensitivity,better thermal stability and high performances. It plays a significant role to replace the current energetic ingredients. In this review,we summarize various strategies involved in the synthesis of NTO as well as the existing approaches to tailor its particle morphology and sizes. The most prominent properties of NTO,such as insensitivity and performance,which are usually required to produce efficient formulations,have been concisely discussed. In addition,this overview reports on some newer forms of NTO including derivatives and co?crystals available in the literature,which can enhance the NTO features and extend its applications. The advantages and shortcomings of various NTO forms for specific and potential use are also highlighted together with the attempts made to overcome these issues. Therefore,efforts will certainly continue to improve characteristics and performances of NTO either by chemical modification or by co?crystallization in order to produce promising formulations for widespread applications in the near future.
基金Supported by the National Natural Science Foundation of China (No. 20962007)the Creative Talents Plan of Hainan University 211 Project
文摘Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2(3H)-carboxamide (1) and N-(2-methoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxamide (2),were synthesized from the initial compound benzo[d]isothiazol-3(2H)-one (BIT) and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.
基金This work was supported by the Natural Science Foundation of Hubei Province (2006ABB016)National Natural Science Foundation of China (20672041) Key Project of Science and Technology of Ministry of Education of China (107082, 106116)
文摘The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4(3H)-one (C16H18N2O3, Mr = 286.32) has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167(14), b = 13.113(1), c = 8.378(1) A, β = 98.992(2)^o, V = 1488.4(3) A^3, Z = 4, Dc = 1.278, F(000) = 608, μ = 0.089 mm^-1, MoKa radiation (2 = 0.71073), R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.
基金support from the Research Council of University of Sistan and Baluchestan, Iran
文摘2,2'-Arylmethylene bis(3-hydroxy-5,5-dimethyl-2-cyclohexene-1-one) 4l-s produced from reaction between dimedone with various aldehydes in acetonitrile using ZnO as a catalyst;whereas in the presence of ZnO-acetyl chloride catalysts the reaction is limited to give only 1,8-dioxo-octahydroxanthenes 3a-k in very good yields.
文摘A new one-pot neat synthesis of some 5-aryl-2,4-dihydro-3H- 1,2,4-triazol-3-ones through cyclocondensation of ethyl carbazate with aryl nitriles catalyzed by DMAP as an efficient and basic nucleophilic catalyst is described.
文摘The synthesis of 3-(2'-hydroxybutyl)isobenzofuran-1(3H)-onel from phthalicanhydride via the intermediate 3-(2'-oxoethyl) isobenzofuran-1(3H)-one 6 was described.
基金financially supported by the National Natural Science Foundation of China(No.21271073)
文摘Solvent extraction of palladium (Ⅱ) from hydrochloric acid solution with 2-n-octyl-4-isothiazolin-3-one (OIT)/cyclohexane was studied. Effects of different parameters on extraction efficiency were evaluated. 99.96 % and 98.26 % palladium (Ⅱ) could be effectively extracted with 0.018 mol·L^-1 OIT/cyclohexane of 0.1 and 4.0 mol·L^-1 HCl medium, respectively. Nonpolar solvent and low acidity could improve the extracting efficiency, and successfully strip palladium (Ⅱ) from the loaded organic phase was achieved with 0.5 mol·L^-1 (NH2)2CS solution. It was proposed that the extraction of Pd com-plexes from HCl medium proceeded through the ion-association mechanism by slope method, NMR and FF-IR spectra.
基金The work was supported by the National Natural Science Foundation of China (29973036)
文摘The single crystal of the title compound (C12H8N2O2, Mr = 212.20) has been obtained by oxidation of 2-aminophenol in methanol solution with irradiation of sunlight. The crystal belongs to monoclinic space group P21/c with cell dimensions of a = 12.925(2), b = 5.077(3), c = 14.768(3)? b = 99.38(1), V = 956.2(5)?, Z = 4, Dc = 1.474 g/cm3, = 0.103 mm-1, R = 0.054, wR = 0.074 for 785 observed reflections (I > 2s(I)). The molecule consists of three coplanar rings. Much different CC distances (1.494(4)?and 1.343(6) ? observed within the quinoidal ring show the pattern of bond fixation expected for the Kekule formula.
文摘Silica-supported tin chloride and titanium tetrachloride were prepared by the reaction of tin chloride and titanium tetrachloride with activated silica gel in refluxing toluene.These solid acids have been employed as the catalysts for the synthesis of bisdihydropyrimidin -2(1H)-ones from aromatic dialdehydes,1,3-dicarbonyl compounds and urea at 90℃under solvent-free conditions.
文摘The title compound C18H16N4O3 (Mr = 336.35) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Schiff base compound is a derivative of 4-aminoantipyrine. As expected, the molecular structure adopts a trans configuration about the central C=N double bond. It crystallizes in orthorhombic, space group P2dc with a = 7.632(1), b = 7.816(1), c = 28.082(5) A,β = 96.18(1)°, V= 1665.48(51) A^3, Z= 4, Dc = 1.341 g/cm^3, F(000) = 704,μ = 0.094 mm^-1, the final R = 0.0448 and wR = 0.1058. Of the total 3748 collections, 3105 were unique. In the molecule there exist two different planes of pyrazoline and C(11)-C(16) phenyl ring, which are approximately coplanar (r.m.s. de deviation from the combined mean plane is 0.03 A) with the dihedral angle between them of 9.8%.
基金Supported by the Natural Science Foundation of Zhejiang Province (2008C21029)
文摘The title compound 3-(2,4-dichlorophenyl)-4-dydroxy-3-(2,4-dichlorophenyl)-4- dydroxy-5-cyclohexanyl-A3-dihydrofuran-2-one 5 has been synthesized by the cyclization of methyl O-(2,4-dichlorophenyl-acetyl)-1-hydroxycyclo-hexane-carboxylate 4, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.8192(3), b = 10.5053(5), c = 10.5811(5)A,α = 71.681(10), β = 78.905(12), γ = 81.036(12)°, C15H14C1203, Mr = 313.18, V= 702.44(6)A3, Z = 2, De= 1.481 g/cm^3, F(000) = 324,μ = 0.465 mm^-1, S = 1.006, the final R = 0.0331 and wR = 0.1363 for 2505 observed reflections with I 〉 2σ(I) and 183 variable parameters. The crystal analysis shows that the cyclohexene unit of the title compound has a quasi-chair conformation, and a one-dimensional chain structure is formed via the intermolecular hydrogen bond O(1)-H(101)…O(2).
基金We gratefully acknowledge financial support of this work by the National Key Project for Basic Research(2003CB114400,2003CB114406)the National Natural Science Foundation of China(Project No.20102001).
文摘Alkylamino-5, 6, 7, 8-tetrahydrobenzothieno [2, 3-d] pyrimidin-4(3H)-ones 7 weresynthesized by a new selective synthetic method, which includes aza-Wittig reaction of imino-phosphorane 4 with aromatic isocynate to give carbodiimide 5 and subsequent reaction of 5 withvarious aliphatic primary amine in the presence of EtO-Na+.
基金Supported by the National Natural Science Foundation of China(No.20962007)Natural Science Foundation of Hainan Province(No.214024)
文摘Twelve Mannich base derivatives of 1,2-benzisothiazolin-3-one were synthesized by the reaction of 1,2-benzisothiazol-3(2H)-one (BIT) with different amines and formaldehyde. All the compounds were characterized by elemental analysis, IR spectroscopy, MS and 1H NMR. The crystal structure for 2,2'-methylenebis(benzo[d]isothiazol-3(2H)-one) (3) has been determined by X-ray single-crystal structure analysis. Compound 3 (C15HIoN202S2) crystallizes in the monoclinic system, space group C2/c with a = 25.052(8), b = 4.510(1), c = 11.948(4) A, β = 100.992(4)°, V= 1325.2(7) A3, Mr = 314.37, Dc = 1.576 Mg.m-3, p = 0.25 mm-1, F(000) = 648, Z = 4, R = 0.034 and wR = 0.087. The preliminary biological test indicated that the compounds (2b, 2c) showed growth inhibitory activity against the gram-positive and gram-negative bacteria.
基金supported by the Medical Research Foundation of Science and Technology of Guangdong Province (No. B2008103)the Natural Science Foundation of Guangdong Province (No. 9451051501002541)
文摘The crystal structure of the title compound 2-ethoxycarbonylmethyl-8-chloro-3a,4-dihydro-3a-methyl-chromeno[4,3-c]pyrazol-3(2H)-one(C15H15ClN2O4,Mr = 322.74) has been prepared and determined by single-crystal X-ray diffraction.The crystal is of orthorhombic,space group Pccn with a = 16.7246(10),b = 19.6626(12),c = 9.3013(6) ,V = 3058.7(3) 3,Z = 8,Dc = 1.402 g/cm3,μ = 0.269 mm-1,F(000) = 1344,the final R = 0.0506 and wR = 0.1464 for 2568 reflections with I 〉 2σ(I).In addition,disordered C(14) and C(15) atoms exist in the crystal structure.