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
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
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
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
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
5,6-Dihydrothieno[3＇,2＇：4,5]thieno[2,3-d]pyrimidin-4（3H）-ones 6 were synthesized in yields of 71-87% by a consecutive method, which includes aza-Wittig reaction of iminophosphorane 3 with aromatic isocynate to gi...5,6-Dihydrothieno[3＇,2＇：4,5]thieno[2,3-d]pyrimidin-4（3H）-ones 6 were synthesized in yields of 71-87% by a consecutive method, which includes aza-Wittig reaction of iminophosphorane 3 with aromatic isocynate to give carbodiimide 4 and subsequent reaction of 4 with various amines, phenols or alcohols in the presence of catalytic amount of sodium ethoxide or solid potassium carbonate. 2009 Ming Wu Ding. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.展开更多
A series of 2,4,5-triaryl substituted 1H-pyrazol-3（2H）-ones,as ALK5 inhibitors,were desigened,synthesized and evaluated in vitro.Most compounds exhibited noticeable ALK5 inhibition activities at 1μmol/L and display...A series of 2,4,5-triaryl substituted 1H-pyrazol-3（2H）-ones,as ALK5 inhibitors,were desigened,synthesized and evaluated in vitro.Most compounds exhibited noticeable ALK5 inhibition activities at 1μmol/L and displayed no significant cytotoxicities at 30μmol/L.展开更多
4,6-Diarylpyrimidin-2(1H)-one derivatives have been synthesized from three-component one-pot condensation of acetophe-none derivatives,aldehydes and urea in the presence of trimethylsilyl chloride and a catalytic amou...4,6-Diarylpyrimidin-2(1H)-one derivatives have been synthesized from three-component one-pot condensation of acetophe-none derivatives,aldehydes and urea in the presence of trimethylsilyl chloride and a catalytic amount of HPMoOunder solvent-free conditions.展开更多
The synthesis of novel isoxazolo[2,3-c][1,3,5]thiadiazepin-2-ones has been achieved in excellent yields by one-pot three-component Domino reaction without the production of toxic waste products by using p-toluene sulf...The synthesis of novel isoxazolo[2,3-c][1,3,5]thiadiazepin-2-ones has been achieved in excellent yields by one-pot three-component Domino reaction without the production of toxic waste products by using p-toluene sulfonic acid (PTSA) as a Lewis acid catalyst. PTSA plays a crucial role in the success of the reaction, as well as for increasing reaction rate.展开更多
Novel 3-phenyl/pyridinyl-trans-2-(aryl/heteryl)vinyl-3H-quinazolin-4-ones 3a,b, 4a, 5a, 7a and their 6,7-difluoro de- rivatives 3c,d, 4b, 5b, 7b have been obtained by condensation of the correspondent 2-methylquinazol...Novel 3-phenyl/pyridinyl-trans-2-(aryl/heteryl)vinyl-3H-quinazolin-4-ones 3a,b, 4a, 5a, 7a and their 6,7-difluoro de- rivatives 3c,d, 4b, 5b, 7b have been obtained by condensation of the correspondent 2-methylquinazolin-4-ones 1, 6 with aromatic (heterocyclic) aldehydes in the presence of ZnCl2 (AcONa) or by the reaction of 2-methyl-3,1-benzoxazin-4- ones 2 with the Shiff bases. Effects of aryl(heteryl) substituents on photophysical properties of (aryl/heteryl) quinazolinylethenes have been studied.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
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
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
The crystal structure of the title compound 1-（4-fluorophenyl） -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H） -one（C23H21FN4O2S,Mr = 436.5） has been prepared and determined by single-cr...The crystal structure of the title compound 1-（4-fluorophenyl） -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H） -one（C23H21FN4O2S,Mr = 436.5） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854（3） ,b = 17.2678（4） ,c = 18.1828（5）A,β = 99.364（2） °,V = 4332.58（18） A^3,Z = 4,Dc = 1.338,F（000） =1824,μ = 0.185 mm^-1,MoKa radiation（λ = 0.71073） ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ（I） . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5（1H） -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.展开更多
The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determin...The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.展开更多
An efficient synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions...An efficient synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions at room temperature by grinding, which provides an efficient route to the synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one.This procedure offers several advantages including solvent-free conditions,excellent yields of products,simple work-up as well as reuse of catalysts which makes it a useful and attractive protocol for the synthesis of these compounds.展开更多
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 synthesis of 3-(2'-hydroxybutyl）isobenzofuran-1(3H)-onel from phthalicanhydride via the intermediate 3-(2'-oxoethyl) isobenzofuran-1(3H)-one 6 was described．
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
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 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.
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.
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.
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support of this work by the National Natural Science Foundation of China(No.20772041)Key Project of Science and Technology of Ministry of Education of China(No.107082)
文摘5,6-Dihydrothieno[3＇,2＇：4,5]thieno[2,3-d]pyrimidin-4（3H）-ones 6 were synthesized in yields of 71-87% by a consecutive method, which includes aza-Wittig reaction of iminophosphorane 3 with aromatic isocynate to give carbodiimide 4 and subsequent reaction of 4 with various amines, phenols or alcohols in the presence of catalytic amount of sodium ethoxide or solid potassium carbonate. 2009 Ming Wu Ding. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.
文摘A series of 2,4,5-triaryl substituted 1H-pyrazol-3（2H）-ones,as ALK5 inhibitors,were desigened,synthesized and evaluated in vitro.Most compounds exhibited noticeable ALK5 inhibition activities at 1μmol/L and displayed no significant cytotoxicities at 30μmol/L.
基金Islamic Azad University of Khorram Abad Council for the financial support
文摘4,6-Diarylpyrimidin-2(1H)-one derivatives have been synthesized from three-component one-pot condensation of acetophe-none derivatives,aldehydes and urea in the presence of trimethylsilyl chloride and a catalytic amount of HPMoOunder solvent-free conditions.
文摘The synthesis of novel isoxazolo[2,3-c][1,3,5]thiadiazepin-2-ones has been achieved in excellent yields by one-pot three-component Domino reaction without the production of toxic waste products by using p-toluene sulfonic acid (PTSA) as a Lewis acid catalyst. PTSA plays a crucial role in the success of the reaction, as well as for increasing reaction rate.
文摘Novel 3-phenyl/pyridinyl-trans-2-(aryl/heteryl)vinyl-3H-quinazolin-4-ones 3a,b, 4a, 5a, 7a and their 6,7-difluoro de- rivatives 3c,d, 4b, 5b, 7b have been obtained by condensation of the correspondent 2-methylquinazolin-4-ones 1, 6 with aromatic (heterocyclic) aldehydes in the presence of ZnCl2 (AcONa) or by the reaction of 2-methyl-3,1-benzoxazin-4- ones 2 with the Shiff bases. Effects of aryl(heteryl) substituents on photophysical properties of (aryl/heteryl) quinazolinylethenes have been studied.
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.
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.
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Supported by the Natural Science Foundation of Hubei Province (2006ABB016)Key Science Research Project of Hubei Provincial Department of Education (No.D200724001)the Science Research Project of Yunyang Medical College (No.2008CXG01)
文摘The crystal structure of the title compound 1-（4-fluorophenyl） -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H） -one（C23H21FN4O2S,Mr = 436.5） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854（3） ,b = 17.2678（4） ,c = 18.1828（5）A,β = 99.364（2） °,V = 4332.58（18） A^3,Z = 4,Dc = 1.338,F（000） =1824,μ = 0.185 mm^-1,MoKa radiation（λ = 0.71073） ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ（I） . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5（1H） -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.
基金Supported by the Central University Basic Scientific Research Fund of Hunan University (2009)the Key Scientific and Technological Project of Changsha, Hunan Province (No. 0901077-31)
文摘The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.
基金supported by the research foundation of Hebei University of Science and Technology
文摘An efficient synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one is achieved via a reaction of acenaphthe-nequinone and indoles catalyzed by solid superacid SO4^2-/TiO2 under solvent-free conditions at room temperature by grinding, which provides an efficient route to the synthesis of symmetrical 2,2-bis（1H-indol-3-yl）-2H-acenaphthen-1-one.This procedure offers several advantages including solvent-free conditions,excellent yields of products,simple work-up as well as reuse of catalysts which makes it a useful and attractive protocol for the synthesis of these compounds.
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.
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.
