屈螺酮关键中间体的合成研究

Study on Synthesis of the Key Intermediate of Drospirenone

以NBS为溴源,3-特戊酰氧基-5β,6β-环氧-7β-羟基-15β,16β-二亚甲基-孕甾-17-酮为原料,在三苯基膦催化剂的作用下合成了屈螺酮的关键中间体3-特戊酰氧基-5β,6β-环氧-7α-溴-15β,16β-二亚甲基-孕甾-17-酮,考察了NBS的用量、催化剂的用量、反应温度、反应时间对3-特戊酰氧基-5β,6β-环氧-7α-溴-15β,16β-二亚甲基-孕甾-17-酮收率的影响。实验结果表明,最佳投料条件下目标物的质量收率为89.5%。该方法条件温和,操作简单,易于实现工业化生产。

With NBS as bromine precursor, and triphenylphosphine as catalysts, 7α-bromo-5,6 β-epoxy-15β,16β-methylene-3β- pivaloyloxy-5β-androstan-17 -one was synthesized from 5,6β-epo -xy-7β-hydroxy-15β,16β-methylene-3β-pivaloyloxy-5β-androstan- 17-one. The effects of the cont- ent of NBS and catalyst, reaction temperatures, reaction time on the reaction yield were discussed in the paper. Under the optimum conditions, the mass yield of target compound was 89.5 %. The method is easy to be industrialized.