Asymmetric synthesis of 3β-acetoxy-17,17-ethylendioxy-15β,16β-methylene-5-androsten-7β-ol

acetoxy-17,17-ethylendioxy-15β,16β-methylene-5-androsten-7β-ol（Ⅰ） was prepared by 3 steps from 3β-acetoxy-15β,16β-methylene-5-androsten-17-one （Ⅱ） with overall yield of 52.7%. Thus, interaction of ethylene glycol and material （Ⅱ） gave 3β-acetoxy- 17,17-ethylendioxy-15β,16β-methylene-5-androsten （Ⅲ） which was subsequently oxidated and stereoselectively reduced to produce compound（Ⅰ）. The normal influencing factors, such as the types of oxidants and reductives, the mole ratio of reactants, the reaction temperature, and the addition ways of reactants, in oxidation and reduction were discussed. The results show that the oxidation rate order is CrO3-C5H5N （1∶1, mole fraction）>CrO3-C5H5N（1∶2）>（C5H5NH）2Cr2O7 in terms of the oxidant, the yield of the oxidation becomes higher with increasing the oxidant stoichiometry and raising the reaction temperature. And the optimum condition is that the reaction temperature is at 30 ℃, and n （Ⅲ）/ n （CrO3-C5H5N（1∶2））=1∶20. The yield of the -7β alcohol order with Li[Al（OC（CH3）3）3H] （e.g.78.6%） is more than that with NaBH4 （e.g.14.5%） in terms of the reductive （agent） and the reduction rate decreases in the course of reaction. The compound （Ⅰ） is characterized by IR and MS.

溪黄草的化学成分研究

目的:对溪黄草的化学成分进行研究。方法:利用萃取,硅胶、凝胶和反相硅胶柱色谱以及高效液相色谱法进行分离和纯化,采用波谱学技术(1D和2D NMR,MS,IR等)进行结构鉴定。结果:分离并鉴定出6个化合物,分别是ent-1α,7α,14β,20-tetrahydroxy-11,16-kauradien-15-one(1),kamebakaurin(2),dihydrokamebakaurin(3),rabdoinflexin A(4),胡萝卜苷(5),β-谷甾醇(6)。结论:其中化合物1为新化合物,化合物3为首次从该植物中分离得到。

雷山石杉的化学成分研究

目的研究雷山石杉的化学成分。方法使用制备薄层、硅胶柱色谱、SephadexLH-20及半制备高效液相色谱法等手段进行分离、纯化，结合文献资料、理化性质、1H—NMR及13C-NMR数据进行结构鉴定。结果分离得到10个化合物，分别鉴定为（15R）-12，16-epoxy-11，14-dihydroxy-8，11，13-abietatrien-7-one（Ⅰ），21-epi—serratenediol-3，21-acetate（Ⅱ），setTatene—diol-3-acetate（Ⅲ），21-epi—serratenediol-3-acetate（Ⅳ），21a—hydroxy—serrat-14-en-3β-ol（Ⅴ），21β-hydroxy—serrat-14-en-3β-ol（Ⅵ），石杉碱甲（huperzineA，Ⅶ），蔗糖（Ⅷ），β-谷甾醇（Ⅸ），胡萝卜串（Ⅹ）。结论化合物Ⅰ～Ⅹ均首次从该植物中分离到。