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
The urinary concentrations of hydroxyproline (HYPRO)and 3 -methyl histidine (3 - MEHIS) were de- termined in 16 Chinese-Holstein cows. The objectives of the experiment were to find out thhe relationship between collag...The urinary concentrations of hydroxyproline (HYPRO)and 3 -methyl histidine (3 - MEHIS) were de- termined in 16 Chinese-Holstein cows. The objectives of the experiment were to find out thhe relationship between collagen and myosin ddegradation and uterine involution in the postpartum cow. The results in the experiment showed that the mean concentrations of HYPRO and 3-MEHIS were 138.32±22.99 and 37.09 ±3.90 nmol·mL-1,respectively,for the cows during the days between 60-90 postpartum,and for the cows immediately after calving the concentrations of HYPRO and 3 -MEHIS reduced from 284.30 and 65.48 nmol ·mL-1 on the day one after calving to the normal level of 109.18 and 33.51 nmol·mL^-1 on the day 50 post- partum,respectively. There was a good correlation between the urinary concentrations of both HYPRO and 3 -MEHIS and the diameters of the involuting uterus (r = 0. 79).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
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 financially by Heilongjiang(C- 9702)and Chinese National (39870572)Natural and Scicntificfunds.
文摘The urinary concentrations of hydroxyproline (HYPRO)and 3 -methyl histidine (3 - MEHIS) were de- termined in 16 Chinese-Holstein cows. The objectives of the experiment were to find out thhe relationship between collagen and myosin ddegradation and uterine involution in the postpartum cow. The results in the experiment showed that the mean concentrations of HYPRO and 3-MEHIS were 138.32±22.99 and 37.09 ±3.90 nmol·mL-1,respectively,for the cows during the days between 60-90 postpartum,and for the cows immediately after calving the concentrations of HYPRO and 3 -MEHIS reduced from 284.30 and 65.48 nmol ·mL-1 on the day one after calving to the normal level of 109.18 and 33.51 nmol·mL^-1 on the day 50 post- partum,respectively. There was a good correlation between the urinary concentrations of both HYPRO and 3 -MEHIS and the diameters of the involuting uterus (r = 0. 79).
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
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.
