3-(4-Chlorophenyl)-7-[2-(piperazin-1-yl)ethoxy]-4H-chromen-4-one(CPEO-43)is a derivative of soybean isoflavone(SI),synthesized by introducing a chlorine atom and a piperazine group into the structure of natural SI.In ...3-(4-Chlorophenyl)-7-[2-(piperazin-1-yl)ethoxy]-4H-chromen-4-one(CPEO-43)is a derivative of soybean isoflavone(SI),synthesized by introducing a chlorine atom and a piperazine group into the structure of natural SI.In vitro experiments have demonstrated that CPEO-43 exhibits a notable inhibitory effect on both A549 cells and HCT116 cells.For the further development and utilization of CPEO-43,this study aims to establish and validate a liquid chromatography-tandem mass spectrometry(LC-MS/MS)quantitative analysis method for the pharmacokinetic study of CPEO-43.Normal rats were intragastrically administered different doses(2,6,and 20 mg/kg)of CPEO-43,and blood was taken from the ocular venous plexus at different time points.The blood concentration of CPEO-43 at different time points was determined using LC-MS/MS technology,and the pharmacokinetic parameters of the compound were calculated using the pharmacokinetic software DAS.The results indicated that the established LC-MS/MS method complies with the standards for bioanalytical method validation in the Chinese Pharmacopoeia(CHP)and can be applied to the pharmacokinetic study of CPEO-43.The pharmacokinetic software DAS non-compartmental model was successfully used to calculate the C_(max),T_(max),t_(1/2),AUC_(0-∞),MRTs,CL,and Vd pharmacokinetic parameters of the compound at different doses.The results were as follows:62.0±10.5,222.0±28.7,and 1384.5±376.4 ng/mL;8.5±1.2,6.0±0.0,and 11.0±6.2 h;15.6,15.0,and 18.5 h;1517.8±317.0,5328.7±864.4,and 45556.3±22735.6 ng·h/mL;17.8±1.2,17.7±0.8,and 20.0±3.2 h;1370.3±305.9,1153.5±205.6,and 505.3±179.8 mL/kg/h;30843.0±7458.0,24344.0±5237.0,and 13950.3±5996.9 mL/kg.These characteristics are of great significance for understanding the in vivo process of the drug,formulating dosing regimens,and evaluating the safety and efficacy of the drug.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
A novel series of compounds combining indolin-2-one and quinazolin-4（3H）-one moiety via a carbon-carbon double bond were synthesized by aldol-condensation of 2-methylquinazolin-4（3H）-one-6-carbaldehyde with variou...A novel series of compounds combining indolin-2-one and quinazolin-4（3H）-one moiety via a carbon-carbon double bond were synthesized by aldol-condensation of 2-methylquinazolin-4（3H）-one-6-carbaldehyde with various indolin-2-ones. The synthesized compounds were evaluated for their cytotoxic activity against five human cancer cell lines, namely, A549, MCF-7, HeLa, HT-29 and HCT-116. We found that compound 5e with two bromine atoms at the 5- and 7-positions of the indolin-2-one ring was most potent, which inhibited proliferation of five cancer cell lines in the range of 32.0%-62.3% at a concentration of 50 p,M. Our results further indicate that the connection of 5,7-dibromoindolin-2-one and 2-methylquinazolin- 4（3H）-one moiety with a carbon-carbon double bond is essential for compound 5e to exert cytotoxicity.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
A series of 1,5-diaryl-1,4-pentadien-3-one derivatives bearing an emodin group were designed and synthesized by the combination of natural products. The antiviral activities against tobacco mosaic virus（TMV） and cuc...A series of 1,5-diaryl-1,4-pentadien-3-one derivatives bearing an emodin group were designed and synthesized by the combination of natural products. The antiviral activities against tobacco mosaic virus（TMV） and cucumber mosaic virus（CMV） in vivo were evaluated. Some of the derivatives displayed promising curative effect and protective activity against TMV. Compound D5 showed appreciable curative bioactivity on TMV approximately of 50% at 306.2 mg/m L, which was superior to ningnanmycin（409.3 mg/m L）.展开更多
A new approach to the facile synthesis of 2-substituted-quinazolin-4（3H）-ones and its derivatives using the condensation reaction of substituted 2-aminobenzamide and orthoesters is reported.
A series of 2,3-dihydroquinazolin-4（1H）-ones have been synthesized in good to excellent yields through direct cyclocondensation of anthranilamide and aryl aldehydes or ketones in water or methanol under mild conditi...A series of 2,3-dihydroquinazolin-4（1H）-ones have been synthesized in good to excellent yields through direct cyclocondensation of anthranilamide and aryl aldehydes or ketones in water or methanol under mild conditions.The reaction was efficiently promoted by 10 mol%sulfamic acid（SA,H_2NSO_3H） and the catalyst could be recovered easily after the reactions and reused without evident loss of reactivity.展开更多
2,3-Dihydroquinazolin-4（1H）-ones have been synthesized in the high to excellent yields via condensation of 2-aminobenzamide with aldehydes and ketones in the presence of catalytic amount of ZrCl_4 in EtOH at room te...2,3-Dihydroquinazolin-4（1H）-ones have been synthesized in the high to excellent yields via condensation of 2-aminobenzamide with aldehydes and ketones in the presence of catalytic amount of ZrCl_4 in EtOH at room temperature.Mild reaction conditions, clean reaction media,simple workup and easy purification are advantages of this methodology.展开更多
Melamine trisulfonic acid（MTSA） can be used as an efficient and recyclable catalyst for the promotion of the synthesis of 3,4- dihydropyrimidin-2（1H）-ones/thiones（DHPMs） in the absence of solvent.All reactions w...Melamine trisulfonic acid（MTSA） can be used as an efficient and recyclable catalyst for the promotion of the synthesis of 3,4- dihydropyrimidin-2（1H）-ones/thiones（DHPMs） in the absence of solvent.All reactions were performed at 80℃in good to high yields.展开更多
To explore new skeleton with nematicidal activity, a series of novel 1,2,3-benzotriazin-4-one derivatives containing piperazine as linker were synthesized and varied fragments were also introduced to increase structur...To explore new skeleton with nematicidal activity, a series of novel 1,2,3-benzotriazin-4-one derivatives containing piperazine as linker were synthesized and varied fragments were also introduced to increase structure diversity of the new skeleton. Their inhibitory activities in vivo were evaluated against Meloidogyne incognita. The newly prepared compounds A6, A8, A21, A28 and A38 exhibited more than 50% inhibition at the concentration of 20 mg/L. Especially compound A6 displayed 71.4% inhibition against Meloidogyne incognita at the concentration of 20 mg/L. The nematicidal activities varied significantly depending on the types and positions of the substituents, which provided guidance for further structure modification.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
A facile one-pot synthesis of 3,4,5-substituted furan-2（5H）-one derivatives from a three-component reaction of aniline derivatives, dialkylacetylenedicarboxylates and aromatic aldehydes under mild conditions using t...A facile one-pot synthesis of 3,4,5-substituted furan-2（5H）-one derivatives from a three-component reaction of aniline derivatives, dialkylacetylenedicarboxylates and aromatic aldehydes under mild conditions using tetra-n-butylammonium bisulfate as a catalyst has been developed.展开更多
A wide range of mono-and disubstituted 2,3-dihydroquinazolin-4（1H）-ones were obtained in high yields by condensation of isatoic anhydride,aldehydes with ammonium salts or primary amines in the presence of strontium ...A wide range of mono-and disubstituted 2,3-dihydroquinazolin-4（1H）-ones were obtained in high yields by condensation of isatoic anhydride,aldehydes with ammonium salts or primary amines in the presence of strontium chloride in aqueous ethanol under reflux.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
An environmentally benign aqueous protocol for the synthesis of 3,4-dihydropyrimidin-2-（ 1 H）-ones and thiones promoted by a green catalyst, silica gel-supported L-pyrrolidine-2-carboxylic acid-4-hydrogen sulfate, h...An environmentally benign aqueous protocol for the synthesis of 3,4-dihydropyrimidin-2-（ 1 H）-ones and thiones promoted by a green catalyst, silica gel-supported L-pyrrolidine-2-carboxylic acid-4-hydrogen sulfate, has been developed. The use of nontoxic, thermally stable and inexpensive amino acid catalyst makes the process simple with minimal amount of chemical waste. Compared with classical Biginelli reaction conditions, this new method has the advantages of high yields and simple workup procedures.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
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
基金Scientific Research Projects of Hebei North University(Grant No.XJ2024022).
文摘3-(4-Chlorophenyl)-7-[2-(piperazin-1-yl)ethoxy]-4H-chromen-4-one(CPEO-43)is a derivative of soybean isoflavone(SI),synthesized by introducing a chlorine atom and a piperazine group into the structure of natural SI.In vitro experiments have demonstrated that CPEO-43 exhibits a notable inhibitory effect on both A549 cells and HCT116 cells.For the further development and utilization of CPEO-43,this study aims to establish and validate a liquid chromatography-tandem mass spectrometry(LC-MS/MS)quantitative analysis method for the pharmacokinetic study of CPEO-43.Normal rats were intragastrically administered different doses(2,6,and 20 mg/kg)of CPEO-43,and blood was taken from the ocular venous plexus at different time points.The blood concentration of CPEO-43 at different time points was determined using LC-MS/MS technology,and the pharmacokinetic parameters of the compound were calculated using the pharmacokinetic software DAS.The results indicated that the established LC-MS/MS method complies with the standards for bioanalytical method validation in the Chinese Pharmacopoeia(CHP)and can be applied to the pharmacokinetic study of CPEO-43.The pharmacokinetic software DAS non-compartmental model was successfully used to calculate the C_(max),T_(max),t_(1/2),AUC_(0-∞),MRTs,CL,and Vd pharmacokinetic parameters of the compound at different doses.The results were as follows:62.0±10.5,222.0±28.7,and 1384.5±376.4 ng/mL;8.5±1.2,6.0±0.0,and 11.0±6.2 h;15.6,15.0,and 18.5 h;1517.8±317.0,5328.7±864.4,and 45556.3±22735.6 ng·h/mL;17.8±1.2,17.7±0.8,and 20.0±3.2 h;1370.3±305.9,1153.5±205.6,and 505.3±179.8 mL/kg/h;30843.0±7458.0,24344.0±5237.0,and 13950.3±5996.9 mL/kg.These characteristics are of great significance for understanding the in vivo process of the drug,formulating dosing regimens,and evaluating the safety and efficacy of the drug.
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National Natural Science Foundation of China (Grant No.20972099,31130017)Beijing Municipal Commission of Education (Grant No.KZ201210028035)+1 种基金Scientific Research Base Development Program of the Beijing Municipal Commission of Educationthe 973 Project (Grant No.2013CB911000)
文摘A novel series of compounds combining indolin-2-one and quinazolin-4（3H）-one moiety via a carbon-carbon double bond were synthesized by aldol-condensation of 2-methylquinazolin-4（3H）-one-6-carbaldehyde with various indolin-2-ones. The synthesized compounds were evaluated for their cytotoxic activity against five human cancer cell lines, namely, A549, MCF-7, HeLa, HT-29 and HCT-116. We found that compound 5e with two bromine atoms at the 5- and 7-positions of the indolin-2-one ring was most potent, which inhibited proliferation of five cancer cell lines in the range of 32.0%-62.3% at a concentration of 50 p,M. Our results further indicate that the connection of 5,7-dibromoindolin-2-one and 2-methylquinazolin- 4（3H）-one moiety with a carbon-carbon double bond is essential for compound 5e to exert cytotoxicity.
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.
基金assistance from the National Natural Science Foundation of China (No. 21302025)the Special Funds for Training object of Outstanding Young Scientific & Technological Talents in Guizhou Province (No. 2015-15#)the Science & Technology Foundation of Guizhou Province (No. J[2014]2056#)
文摘A series of 1,5-diaryl-1,4-pentadien-3-one derivatives bearing an emodin group were designed and synthesized by the combination of natural products. The antiviral activities against tobacco mosaic virus（TMV） and cucumber mosaic virus（CMV） in vivo were evaluated. Some of the derivatives displayed promising curative effect and protective activity against TMV. Compound D5 showed appreciable curative bioactivity on TMV approximately of 50% at 306.2 mg/m L, which was superior to ningnanmycin（409.3 mg/m L）.
基金the Natural Science Foundation of China(Nos.U0832005,90813011,20772159,30801436)the Ministry of Education of the People's Republic of China(No.200805581163)+1 种基金the Guangdong Natural Science Foundation(No.8451008901000214)the Science Foundation of Guangzhou(No.2009A1-E011-6)for financial support of this study.
文摘A new approach to the facile synthesis of 2-substituted-quinazolin-4（3H）-ones and its derivatives using the condensation reaction of substituted 2-aminobenzamide and orthoesters is reported.
文摘A series of 2,3-dihydroquinazolin-4（1H）-ones have been synthesized in good to excellent yields through direct cyclocondensation of anthranilamide and aryl aldehydes or ketones in water or methanol under mild conditions.The reaction was efficiently promoted by 10 mol%sulfamic acid（SA,H_2NSO_3H） and the catalyst could be recovered easily after the reactions and reused without evident loss of reactivity.
文摘2,3-Dihydroquinazolin-4（1H）-ones have been synthesized in the high to excellent yields via condensation of 2-aminobenzamide with aldehydes and ketones in the presence of catalytic amount of ZrCl_4 in EtOH at room temperature.Mild reaction conditions, clean reaction media,simple workup and easy purification are advantages of this methodology.
基金the University of Guilan Research Council for the partial support of this work
文摘Melamine trisulfonic acid（MTSA） can be used as an efficient and recyclable catalyst for the promotion of the synthesis of 3,4- dihydropyrimidin-2（1H）-ones/thiones（DHPMs） in the absence of solvent.All reactions were performed at 80℃in good to high yields.
基金financial supported by the National Natural Science Foundation of China(No. 21672061)National Key Research Program of China(Nos.2017YFD0200505 and 2018YFD0200105)the Fundamental Research Funds for the Central Universities(No. 222201718004)
文摘To explore new skeleton with nematicidal activity, a series of novel 1,2,3-benzotriazin-4-one derivatives containing piperazine as linker were synthesized and varied fragments were also introduced to increase structure diversity of the new skeleton. Their inhibitory activities in vivo were evaluated against Meloidogyne incognita. The newly prepared compounds A6, A8, A21, A28 and A38 exhibited more than 50% inhibition at the concentration of 20 mg/L. Especially compound A6 displayed 71.4% inhibition against Meloidogyne incognita at the concentration of 20 mg/L. The nematicidal activities varied significantly depending on the types and positions of the substituents, which provided guidance for further structure modification.
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fnancial support from the Research Council of the University of Sistan and Baluchestan
文摘A facile one-pot synthesis of 3,4,5-substituted furan-2（5H）-one derivatives from a three-component reaction of aniline derivatives, dialkylacetylenedicarboxylates and aromatic aldehydes under mild conditions using tetra-n-butylammonium bisulfate as a catalyst has been developed.
文摘A wide range of mono-and disubstituted 2,3-dihydroquinazolin-4（1H）-ones were obtained in high yields by condensation of isatoic anhydride,aldehydes with ammonium salts or primary amines in the presence of strontium chloride in aqueous ethanol under reflux.
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Financial support to this work by the Ilam University,Ilam,Iran is gratefully acknowledged
文摘An environmentally benign aqueous protocol for the synthesis of 3,4-dihydropyrimidin-2-（ 1 H）-ones and thiones promoted by a green catalyst, silica gel-supported L-pyrrolidine-2-carboxylic acid-4-hydrogen sulfate, has been developed. The use of nontoxic, thermally stable and inexpensive amino acid catalyst makes the process simple with minimal amount of chemical waste. Compared with classical Biginelli reaction conditions, this new method has the advantages of high yields and simple workup procedures.
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.
