The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in eth...The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis＇ Crystallographic data： C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672（3）, b = 0.66383（12）, c = 1.1617（2） nm, β = 109.275（2）°, V = 1.2136（4） nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F（000） = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.展开更多
The title compound cinobufagin 3-hemisuberate methyl ester（1） was isolated from the venom of Bufo bufo gargarizans CANTOR. The crystal structure of 1, C35H48O9, was determined by single-crystal X-ray diffraction ana...The title compound cinobufagin 3-hemisuberate methyl ester（1） was isolated from the venom of Bufo bufo gargarizans CANTOR. The crystal structure of 1, C35H48O9, was determined by single-crystal X-ray diffraction analysis. It belongs to orthorhombic, space group P212121 with a = 8.9338（3）, b = 16.2970（4）, c = 22.4019（6） , V = 3261.59（16） 3, Mr = 612.73, Z = 4, Dc = 1.248 g/cm3, μ = 0.725 mm-1, F（000） = 1320, S = 1.040, the final R = 0.0374 and wR = 0.0412 for 4458 unique reflections, of which 4088 were observed（I 〉 2σ（I））. In the solid state, short intermolecular C-H...O interactions involving a methine and the ester carbonyl group in cinobufagin moiety and a methyl in the suberate moiety linked adjacent molecules into a three-dimensional network. Detailed analysis of the 1H-NMR data showed that X-ray structure of 1 would be expected to closely resemble the solution conformation in chloroform. Compound 1 was inactive for the inhibition of PC3 and HepG2 cancer cells, but the parent compound cinobufagin showed potent inhibition with IC50 values of 0.145 and 5.48 μM, respectively, indicating that esterification at C（3） decreased the cytotoxic effect of 1.展开更多
4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single ...4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.展开更多
A new compound. methyl 4. 6-O-benzylidene-a-D-glucopyranoside 2. 3-cyclicphosphite ethyl ester was synthesized via the reaction of methyl 4. 6-O-benzylidene-a-D-glucopyranoside and ethyl dichlorophosphite. Its structu...A new compound. methyl 4. 6-O-benzylidene-a-D-glucopyranoside 2. 3-cyclicphosphite ethyl ester was synthesized via the reaction of methyl 4. 6-O-benzylidene-a-D-glucopyranoside and ethyl dichlorophosphite. Its structure was confirmed by NMR and MSspectral methods.展开更多
The synthesis of 99-acetoxy-3(4), 11(13)-dien-5αH 7αH-12-eudesmanoic acid methyl ester (2) was achieved from oxycarvone. The key step is the p-toluenesulfonhydrazide assisted reductiv rearrangement reaction
As the biodiesel production is rapidly enhanced, the crude glycerol, which is by-product of biodiesel processes, is state of surplus. 1,3-PDO (1,3-propanediol), a valuable monomer of poly(trimethylene terephthalate) (...As the biodiesel production is rapidly enhanced, the crude glycerol, which is by-product of biodiesel processes, is state of surplus. 1,3-PDO (1,3-propanediol), a valuable monomer of poly(trimethylene terephthalate) (PTT), can be produced from the fermentation process using crude glycerin as a carbon source. For the economic biological production of 1,3-PDO, the low cost and high efficient separation processes is essential. In this study, aqueous two-phase system composed of various hydrophilic alcohols and salt was used as a primary separation step for 1,3-PDO. It was found that the aqueous two-phase systems are easily formed with decreasing of the polarity of alcohols. The extraction efficiency is proportional to the polarity of alcohols. In case of methanol or ethanol/K2HPO4, the extraction efficiency was more than 90%.? It was concluded that the aqueous two-phase extraction using methanol or ethanol/K2HPO4 can be applied? for the primary separation of 1,3-PDO? as an alternative to a conventional primary separation processes.展开更多
1,3-Propanediol is a promising renewable resource produced by microbial production. It is mainly used in many synthetic reactions, particularly applied to the polymer synthesis and cosmetics industry. We described her...1,3-Propanediol is a promising renewable resource produced by microbial production. It is mainly used in many synthetic reactions, particularly applied to the polymer synthesis and cosmetics industry. We described here the isolation of strain ZH-1, which has the ability of high production with 1,3-propanediol, from Fenhe River in China. It was classified as a member of K. pneumoniae after the study of phenotypic, physio-logical, biochemical and phylogenetic (16S rDNA). The initial glycerol concentration, fermentation time and pH value of strain ZH-1 were determined to be 50 g·L<sup>-1</sup>, 36 h and 8.0. Under these conditions, the practical yield of 1,3-PD was 18.53 g·L<sup>-1</sup> and a molar yield (mol<sub>1,3-PD</sub> mol<sub>Glycerol</sub>-1</sup> of 1,3-propanediol to glycerol of 0.497. In addition, we found that for the strain ZH-1, the optimum grown pH was 9.0, so we can deter-mine that it is a new member of alkali-resistant strains.展开更多
The natural environment is inhabited by many species that exhibit very specific metabolic activities that may find industrial applications. The aim of the study was to select non-pathogenic cultures of bacteria of the...The natural environment is inhabited by many species that exhibit very specific metabolic activities that may find industrial applications. The aim of the study was to select non-pathogenic cultures of bacteria of the genus Clostridium and lactic acid bacteria able to convert glycerol into 1,3-propanediol (1,3-PD). Another aim of this study was to identify the isolates that best produced 1,3-propanediol both from pure and crude glycerol. The most efficient strains identified (Cl. butyricum) were analysed on a bioreactor scale. The aim was to determine temperature conditions on the efficiency and duration of 1,3-PD synthesis. The species Clostridium were identified using amplification of the 16S rRNA coding sequence. A total of 123 isolates (of the genus Clostridium and lactic acid bacteria) were isolated;a vast majority of these were able to synthesize 1,3-PD. The best results were obtained for Cl. butyricum strain DSP1, which was isolated from the rumen of a cow fed with glycerol. The strain efficiency using pure glycerol on bioreactor scale 0.65 mol/mol of glycerol at a temperature of 38℃ and a constant pH of 7.0.展开更多
The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-（4-quinoxalin- 2-yl-phenoxy）-tetrahydro-pyran-4-yl-ester 8 （C28H28N2O10, Mr = 552.54）, has been synthesized and its crystal structure was determined ...The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-（4-quinoxalin- 2-yl-phenoxy）-tetrahydro-pyran-4-yl-ester 8 （C28H28N2O10, Mr = 552.54）, has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21, a = 10.060（8）, b = 5.648（4）, c = 24.11（2）A, β = 91.078（10）°, Z = 2, V= 1369.9（19）A^3, Dc = 1.339 g/cm^3,μ（MoKa） = 1.03 cm^-1, F（000） = 580.00, T =. 193.1 Kx-9 θmax = 25.03, （△/σ）max = 0.0000, Flack = -0.0（24）, the final R = 0.0680 and wR = 0.140 （w = 1/[0.0016Fo^2 ＋ 1.00000（Fo^2）]/（4Fo^2）） for 3126 observed reflections （1 〉 20（/））. The pyranoid ring adopts chair conformation in the sugar moiety, and all of the acetyl groups are in the e bond of the pyranoid ring, so the sugar moiety is very stable.展开更多
基金This work was supported by the National Natural Science Foundation of China (20571060) and Education Committee of Shaan Xi Province (05JK294)
文摘The title compound 4-（4,6-dimethoxylpyrimidin-2-yl）-3-thiourea carboxylic acid methyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at the room temperature. The structure was characterized by elemental analysis and IR and determined by X-ray diffraction analysis＇ Crystallographic data： C9H12N4O4S, Mr = 272.29, monoclinic, space group C2/m with a = 1.6672（3）, b = 0.66383（12）, c = 1.1617（2） nm, β = 109.275（2）°, V = 1.2136（4） nm^3, Dc = 1.490 g/cm^3,μ = 0.281 mm^-1, F（000） = 568, Z = 4, R1 = 0.0341and wR2 = 0.1042.
基金supported by the National Natural Science Foundation of China(81102518)
文摘The title compound cinobufagin 3-hemisuberate methyl ester（1） was isolated from the venom of Bufo bufo gargarizans CANTOR. The crystal structure of 1, C35H48O9, was determined by single-crystal X-ray diffraction analysis. It belongs to orthorhombic, space group P212121 with a = 8.9338（3）, b = 16.2970（4）, c = 22.4019（6） , V = 3261.59（16） 3, Mr = 612.73, Z = 4, Dc = 1.248 g/cm3, μ = 0.725 mm-1, F（000） = 1320, S = 1.040, the final R = 0.0374 and wR = 0.0412 for 4458 unique reflections, of which 4088 were observed（I 〉 2σ（I））. In the solid state, short intermolecular C-H...O interactions involving a methine and the ester carbonyl group in cinobufagin moiety and a methyl in the suberate moiety linked adjacent molecules into a three-dimensional network. Detailed analysis of the 1H-NMR data showed that X-ray structure of 1 would be expected to closely resemble the solution conformation in chloroform. Compound 1 was inactive for the inhibition of PC3 and HepG2 cancer cells, but the parent compound cinobufagin showed potent inhibition with IC50 values of 0.145 and 5.48 μM, respectively, indicating that esterification at C（3） decreased the cytotoxic effect of 1.
基金supported by the National Natural Science Foundation of China (20571060)Natural Science Foundation of Shaanxi Province (2007B08)Education Committee of Shaanxi Province (05JK294)
文摘4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.
文摘A new compound. methyl 4. 6-O-benzylidene-a-D-glucopyranoside 2. 3-cyclicphosphite ethyl ester was synthesized via the reaction of methyl 4. 6-O-benzylidene-a-D-glucopyranoside and ethyl dichlorophosphite. Its structure was confirmed by NMR and MSspectral methods.
文摘The synthesis of 99-acetoxy-3(4), 11(13)-dien-5αH 7αH-12-eudesmanoic acid methyl ester (2) was achieved from oxycarvone. The key step is the p-toluenesulfonhydrazide assisted reductiv rearrangement reaction
文摘As the biodiesel production is rapidly enhanced, the crude glycerol, which is by-product of biodiesel processes, is state of surplus. 1,3-PDO (1,3-propanediol), a valuable monomer of poly(trimethylene terephthalate) (PTT), can be produced from the fermentation process using crude glycerin as a carbon source. For the economic biological production of 1,3-PDO, the low cost and high efficient separation processes is essential. In this study, aqueous two-phase system composed of various hydrophilic alcohols and salt was used as a primary separation step for 1,3-PDO. It was found that the aqueous two-phase systems are easily formed with decreasing of the polarity of alcohols. The extraction efficiency is proportional to the polarity of alcohols. In case of methanol or ethanol/K2HPO4, the extraction efficiency was more than 90%.? It was concluded that the aqueous two-phase extraction using methanol or ethanol/K2HPO4 can be applied? for the primary separation of 1,3-PDO? as an alternative to a conventional primary separation processes.
文摘1,3-Propanediol is a promising renewable resource produced by microbial production. It is mainly used in many synthetic reactions, particularly applied to the polymer synthesis and cosmetics industry. We described here the isolation of strain ZH-1, which has the ability of high production with 1,3-propanediol, from Fenhe River in China. It was classified as a member of K. pneumoniae after the study of phenotypic, physio-logical, biochemical and phylogenetic (16S rDNA). The initial glycerol concentration, fermentation time and pH value of strain ZH-1 were determined to be 50 g·L<sup>-1</sup>, 36 h and 8.0. Under these conditions, the practical yield of 1,3-PD was 18.53 g·L<sup>-1</sup> and a molar yield (mol<sub>1,3-PD</sub> mol<sub>Glycerol</sub>-1</sup> of 1,3-propanediol to glycerol of 0.497. In addition, we found that for the strain ZH-1, the optimum grown pH was 9.0, so we can deter-mine that it is a new member of alkali-resistant strains.
文摘The natural environment is inhabited by many species that exhibit very specific metabolic activities that may find industrial applications. The aim of the study was to select non-pathogenic cultures of bacteria of the genus Clostridium and lactic acid bacteria able to convert glycerol into 1,3-propanediol (1,3-PD). Another aim of this study was to identify the isolates that best produced 1,3-propanediol both from pure and crude glycerol. The most efficient strains identified (Cl. butyricum) were analysed on a bioreactor scale. The aim was to determine temperature conditions on the efficiency and duration of 1,3-PD synthesis. The species Clostridium were identified using amplification of the 16S rRNA coding sequence. A total of 123 isolates (of the genus Clostridium and lactic acid bacteria) were isolated;a vast majority of these were able to synthesize 1,3-PD. The best results were obtained for Cl. butyricum strain DSP1, which was isolated from the rumen of a cow fed with glycerol. The strain efficiency using pure glycerol on bioreactor scale 0.65 mol/mol of glycerol at a temperature of 38℃ and a constant pH of 7.0.
基金This project was supported by the Key Laboratory of Organic Synthesis of Jiangsu Province
文摘The title compound, acetic acid-3,5-diacetoxy-2-acetoxymethyl-6-（4-quinoxalin- 2-yl-phenoxy）-tetrahydro-pyran-4-yl-ester 8 （C28H28N2O10, Mr = 552.54）, has been synthesized and its crystal structure was determined by X-ray diffraction analysis. It crystallizes in monoclinic, space group P21, a = 10.060（8）, b = 5.648（4）, c = 24.11（2）A, β = 91.078（10）°, Z = 2, V= 1369.9（19）A^3, Dc = 1.339 g/cm^3,μ（MoKa） = 1.03 cm^-1, F（000） = 580.00, T =. 193.1 Kx-9 θmax = 25.03, （△/σ）max = 0.0000, Flack = -0.0（24）, the final R = 0.0680 and wR = 0.140 （w = 1/[0.0016Fo^2 ＋ 1.00000（Fo^2）]/（4Fo^2）） for 3126 observed reflections （1 〉 20（/））. The pyranoid ring adopts chair conformation in the sugar moiety, and all of the acetyl groups are in the e bond of the pyranoid ring, so the sugar moiety is very stable.
