摘要
目的研究奥贝胆酸关键双键杂质的合成方法。方法以鹅去氧胆酸甲酯为起始原料,通过上TMS保护剂、羟醛缩合、水解和还原反应等步骤得到奥贝胆酸双键杂质——(Z)-3α,7α-二羟基-6-亚乙基-5β-胆烷酸(A-1)。结果与结论经1H NMR、13C NMR和HRMS确证了化合物的结构,纯度达97.2%(示差检测器)。本研究方法可合成纯度较高的奥贝胆酸杂质A-1,可用于奥贝胆酸的质量研究。
Objective To study the synthetic method for the key double bond impurity of obeticholic acid.Methods Obeticholic acid double bond impurity(Z)-3α,7α-dihydroxy-6-ethylidene-5β-cholanoic acid(A-1) was obtained through the steps of applying TMS protective agent,aldol condensation,hydrolysis and reduction reaction by using methyl chenodeoxycholate as the starting material.Results and Conclusion The structure of synthesized A-1 has been confirmed by 1 H NMR,13C NMR and HRMS with high purity,which can be used for quality research of obeticholic acid.
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
《广东药科大学学报》
CAS
2021年第2期63-65,共3页
Journal of Guangdong Pharmaceutical University
基金
广东省医学科学技术基金项目(B2019003)。
关键词
奥贝胆酸
杂质
合成
obeticholic acid
impurity
synthesis
