甲泼尼龙关键中间体的合成工艺研究

Study on Synthesis Technology of Key Intermediates of Methylprednisolone

以17α-羟基孕甾-4-烯-3,11,20-三酮作为起始原料,经缩酮保护、NaBH4还原、间氯过氧苯甲酸(m-CPBA)环氧化、格氏反应、水解、消除等步骤制备得到甲泼尼龙关键中间体6α-甲基氢化产物。其中,格氏反应、水解、消除等步骤无需分离,操作简单、反应温和,且对环境友好,反应总收率达54%。

Using 17α-hydroxypregna-4-ene-3,11,20-trione as the starting material,the key intermediates of methylprednisolone(6α-methyl hydride)were prepared through ketal protection,NaBH4 reduction,m-CPBA epoxidation,Grignard reaction,hydrolysis,elimination and other steps.Among them,the steps of Grignard reaction,hydrolysis and elimination do not need to be separated,the operation is simple,the reaction is mild,and it is environmentally friendly,and the total reaction yield reaches 54%.