21-氯代氢化可的松的合成工艺改进
Improvement of Synthetic Process of 21-Hydrocortisone Chloride
雷伟 1陈益俊 1徐杰 1于旭超1
作者信息
- 1. 台州仙琚药业有限公司,浙江 台州 317016
- 折叠
摘要
针对现有工艺制备21-氯代氢化可的松存在成本较高、试剂毒性大等问题,采用9-羟基雄烯二酮作为原料,经氰基化、消除、硅醚化及重排4步反应制备得到21-氯代氢化可的松,考察了各步骤的反应条件并得到较优的工艺路线,采用核磁、质谱数据表征了产物结构.实验结果表明,该方法具有原料价廉易得、生产成本低及三废排放量少等优点,总收率可达66.9%,适用于工业化放大.
Abstract
Considering the issues of high cost and high toxicity of reagents in the current process for synthesizing 21-chlorohydrocortisone,9-hydroxy-androstenedione was used as raw material to prepare 21-hydrocortisone chloride by four steps of cyanidation,elimination,silotheration and rearrangement.The reaction conditions of each step were investigated and the optimal process route was obtained.The structure of the product was characterized by NMR and MS data.The experimental results show that the method has the advantages of cheap raw materials,low production cost and less discharge of three wastes.The total yield can reach 66.9%,which is suitable for industrial amplification.
关键词
9-羟基雄烯二酮/21-氯氢化可的松/氰醇化/重排反应Key words
9-hydroxandrostenedione/21-chlorohydrocortisone/cyanohydrintion/rearrangement reaction引用本文复制引用
出版年
2024
NETL
NSTL
万方数据