Synthesis and Crystal Structure of 4-(4,6-dimethoxyl -pyrimidin-2-yl)-3-thiourea Carboxylic Acid Methyl Ester

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.

Synthesis and Crystal Structure of 2-[(4-Methoxy- 6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl] Benzoic Acid Methyl Ester

The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amine with 2-methoxylcarbonylbenzene-sulfonylisocya- nate. The crystal is of monoclinic, space group P21/c with a =11.169(3), b = 9.508(3), c = 17.690(5) ? b = 91.593(5), Z = 4, V = 1877.9(10) 3, Dc = 1.459 g/cm3, F(000) = 856, m(MoKa) = 0.324 mm-1, R = 0.0690 and wR = 0.1368 for 3301 observed reflections (I > 2s(I)). The N(1)H…N(3) and N(2)H…O(4) hydrogen bonds can be observed. In the molecule the phenyl plane(I), pyrimi- din-2-yl-urea bridge plane(Ⅱ) and ester plane(Ⅲ) form three conjugated systems.

Synthesis and Crystal Structure of 4-(4,6-Dimethoxylpyrimidin-2-yl)-3-thiourea Carboxylic Acid Ethyl Ester

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.

2-(4-溴甲基苯基)丙酸及其酯的合成

以对甲苯苯乙腈为原料经甲基化、水解和溴代3步反应合成了2-(4-溴甲基苯基)丙酸和以对甲基苯乙酸乙酯为原料经甲基化和溴代两步合成2-(4-溴甲基苯基)丙酸乙酯。重点探讨了甲基化反应的反应时间及不同相转移催化剂聚乙醇(PEG)对反应的影响。实验结果表明,甲基化反应以8 h为宜,对甲基苯乙腈和对甲苯苯乙酸乙酯甲基化反应的最佳温度分别为180和220℃,前者以碳酸钾与PEG-400共同催化效果较佳,后者以碳酸钾与PEG-600共同催化效果较佳。该两种合成方法收率分别为67.6%和74.8%。

RP-HPLC梯度淋洗法测定一步法合成抗氧剂1010的组分

本文报道采用RP-HPLC梯度淋洗法测定一步法合成抗氧剂1010的组分,色谱分离出十一个特征吸收峰。用外标法和内标法定量对比,其各组分的回:收率为94.51～100.82%,灵敏度为0.49～3.21μg,变异系数在0.80～1.91%范围内。本法准确、灵敏,可满足科研和工业生产的定量分析要求。

Constituents from the Roots of Semiaquilegia adoxoides

In present literature search, some cyano-containing compounds, which are very rare in plants, from the traditional anticancer herb Tiankuizi were reported. To find more cyano-containing compounds in the important plant Semiaquilegia adoxoides （DC） Makino （Chinese name Tiankuizi）, the isolation of the chemical constituents was investigated for advancing the research. Two new compounds, a new alkaloid, 1,2,3,4-tetrahydro-6-hydroxy-1[（3,4-dihydroxyphenyl）methyl]-7-methoxy-2,2-dimethyl-isoquinolinium, named Semiaquilegine A （1）, and a new ester, 3-（4＇-hydroxyphenyl）-2-propenoic acid （4＂-carboxyl）-phenyl ester （2）, and four cyano-containing compounds, （Z）-6a-（β-D-glucosyloxy）-4a,5a-dihydroxy-2-cyclohexene-△^1,a-acetonitrile （3）, （L0-6α-（β-D-glucosyloxy）-4α-hydroxy-2-cyclohexene-△^1,α-acetonitrile （4）, lithospermoside （5）, ehretioside B （6）, as well as eleven known compounds, were isolated from the roots of Semiaquilegia adoxoides. The structures of new compounds 1 and 2 were elucidated mainly by 1D/2D-NMR techniques. Very unusual cyano-containing compounds 3 and 4 were first isolated from Ranunculaceae family. Hitherto, there were six cyano-containing compounds found in the herb.

A New Phenylated Flavone from Melicope pteleifolia

Objective To study the constituents in Melicope pteleifolia.Methods Plant material was isolated with 80% EtOH.Compounds were separated with chromatographic methods and their structures were elucidated on the basis of spectral analysis(EI-MS,1H-NMR,and 13C-NMR) and chemical evidence.Results Five compounds were isolated from petrol ether or ethyl acetate soluble fraction.Their structures were identified as 3,5,3’-trihydroxy-4’-methoxy-7-(3-methylbut-2-enyloxy) flavone(pteleifolosin C,1),3,7-dimethoxyl kaempferol(kamatakenin,2),vanillic acid(3),tricosanoic acid tetradecyl ester(4),and β-sitosterol(5),respectively.Conclusion Compound 1 is a new structure named pteleifolosin C.Compounds 2-4 are isolated from this plant for the first time.

HPLC法测定安立生坦片中有关物质

目的:建立高效液相色谱法测定安立生坦片中有关物质。方法:采用安捷伦ZORBAX SB-Aq(4.6mm×250 mm,5μm)色谱柱,流动相A为5 mmol·L^(-1)磷酸二氢钾溶液(p H 3.0),流动相B为乙腈,以1.0m L·min^(-1)的流速进行梯度洗脱,检测波长为210 nm,柱温25℃,以自身对照法测定安立生坦片中有关物质。结果:安立生坦与各杂质及降解产物能够完全分离(分离度大于2.0);供试品溶液在24 h内稳定性良好;安立生坦和2-羟基-3-甲氧基-3,3-二苯基丙酸(杂质A)、(S)-1-(4-氯苯基)乙胺(杂质B)、3,3二苯基-2,3-环氧丙酸甲酯(杂质C)、2-羟基-3-甲氧基-3,3二苯基丙酸甲酯(杂质D)、4,6-二甲基-2-甲基-磺酰嘧啶(杂质E)和4,6-二甲基-2-(2,2-二苯基-乙烯氧基)嘧啶(杂质F)的定量限分别为0.66、0.64、0.65、1.31、0.65、0.63和1.32 ng,相对校正因子分别为1.00、1.08、2.20、1.09、1.10、2.54和1.07;安立生坦质量浓度在0.5~5.0μg·m L^(-1)范围内线性良好(r>0.999 9),各杂质质量浓度在0.125~2.5μg·m L^(-1)范围内线性良好(r>0.999),杂质加样回收率(n=9)在95.8%～103.7%之间;重复性和中间精密度符合规定。经检测,3批安立生坦片中杂质A含量均为0.01%。结论:经验证本方法准确、灵敏,精密度高,耐用性和专属性强,可用于安立生坦片中有关物质的测定。