一种地塞米松关键中间体的合成方法

A Method for Synthesis of Key Intermediate of Dexamethasone

介绍了一种以16α-甲基-9-脱氢雄烯二酮作为起始原料,制备地塞米松关键中间体9,11α-环氧-16α-甲基-17α-羟基-21-氯代黄体酮的方法。该过程经历了氰醇化、醚化、重排、环氧化五步反应,操作方法简单,优化后的总收率可达61%,产物结构经1H NMR,13C NMR及MS(ESI)确证。

A method for preparing dexamethasone key intermediate 9,11α-epoxy-16α-methyl-17α-hydroxy-21-chloroprogesterone with 16α-methyl-9-dehydroandrostenedione as starting material was introduced.The process underwent five-step reactions of cyanohydrination,etherification,rearrangement and epoxidation.The method is simple to operate and the optimized total yield can increase to 61%.The structure of product is confirmed by1 H NMR,13 C NMR and MS(ESI).