摘要
以(Z)-6-亚乙基-鹅去氧胆酸为原料,经氢气钯碳还原烯烃、硼氢化钠还原羰基,得到奥贝胆酸关键异构体杂质6β-乙基-鹅去氧胆酸(OCA-β),两步产率分别为46%和78%。使用1H NMR、^(13)C NMR、HRMS等确证其结构。该方法具有操作简单、反应条件温和、产率高等优点。
The key epimer impurity obeticholic acid,6β-ethyl-chenodeoxycholic acid(6β-OCA),was synthesized by using(Z)-6-ethylidene-chenodeoxycholic acid as starting material via the reaction of reduction by Pd/C and sodium borohydride with the yield of 46%and 78%,respectively.The structure of epimer impurity was confirmed by 1H NMR,^(13)C NMR and HRMS.This research method possessed several advantages such as simple operation,mild reaction condition and high yield.
作者
张尚师
郑滔
谢晓玲
邓南翔
舒兵
Zhang Shangshi;Zheng Tao;Xie Xiaoling;Deng Nanxiang;Shu Bing(Center for Drug Research and Development,Guangdong Pharmaceutical University,Guangzhou 510006,China;School of Pharmacy,Guangdong Pharmaceutical University,Guangzhou 510006,China)
出处
《山东化工》
CAS
2021年第14期13-14,共2页
Shandong Chemical Industry
基金
广东省医学科学技术基金项目(B2019003)。
关键词
奥贝胆酸
异构体杂质
合成
obeticholic acid
epimer impurity
synthesis
