摘要
以雄烯二酮为原料,经3,17位亚乙二氧基化,7位烯丙位氧化合成了目标化合物3,3,17,17-亚乙二氧基-7-羰基-雄烯二酮,总收率为45.2%。目标化合物和中间体的结构经IR,1 H NMR和MS确证。3,3,17,17-亚乙二氧基-7-羰基-雄烯二酮烯丙位氧化的最佳合成条件如下:n(PDC)∶n(t-BuOOH)∶n(3,3,17,17-亚乙二氧基-雄烯二酮)=4∶4∶1,反应温度为25℃,反应时间为5h。此合成方法反应原料易得,反应条件温和且产率高。
The title compound 3, 3, 17, 17- bis （ethylenedioxy）-androsten-7-one was synthesized from androstenedione by acetalization of 3, 17-carbonyl groups and oxydation of 7-methylene. The target product and intermediates were identified by IR, I H NMR and MS. The total yield of the title compound was 45.2%, which was obtained under optimized conditions： n（PDC） -： n（t-BuOOH） ： n（3,3,17,17- bis（ethylenedioxy）-androstenedi-one）= 4 ： 4 ： 1, reaction temperature of 25 ℃ and reaction time of 5 h. This method has such advantages of mild condition, simple operation and high yield.
出处
《河北工业科技》
CAS
2012年第6期370-372,375,共4页
Hebei Journal of Industrial Science and Technology
