以去氢表雄酮(DHEA)为原料,经过3位羟基乙酰化、17位羰基亚乙二氧基化和烯丙位氧化合成了3β-乙酰氧基-17,17-亚乙二氧基-5-雄甾烯-7-酮,目标化合物和中间体的结构经IR1、HNMR和MS确证。考察了不同氧化剂、反应温度、反应时间对产品收率的影响。确定了最佳反应条件:以n(PDC)∶n(t-BuOOH)∶n(3β-乙酰氧基-17,17-亚乙二氧基-5-雄甾烯)=4∶4∶1,反应温度25℃,反应时间8 h,总收率达57.9%。该路线反应条件温和、操作简单且产率高。 The 3β-acetoxy-17,17-ethylenedioxy group was synthesized from dehydroepiandrosterone (DHEA) through 3-hydroxyacetylation, 17-carbonylethylenedioxylation and allylic oxidation -5-androsten-7-one, the structures of the target compounds and intermediates were confirmed by IR1, HNMR and MS. The effects of different oxidants, reaction temperature and reaction time on the yield of the product were investigated. The optimal reaction conditions were as follows: n (PDC): n (t-BuOOH): n (3β-acetoxy-17,17-ethylenedioxy- , The reaction temperature was 25 ℃, the reaction time was 8 h and the total yield was 57.9%. The route has mild reaction conditions, simple operation and high yield.