摘要
以易得的中间体5为原料,合成了5个奥贝胆酸关键中间体杂质,分别为6-β-乙基-7-酮石胆酸(A)、6-β-乙基-7-酮-石胆酸甲酯(B)、3-α-乙酰基-6-β-乙基-7-酮石胆酸(C)、6-α-乙基-7-酮-石胆酸甲酯(D)、3-α-乙酰基-6-α-乙基-7-酮-石胆酸(E),其结构经^(1)H NMR、^(13)C NMR和HR-MS确证。并通过单晶确定了杂质A的构型,进一步确认了化合物的结构。
The 5 key intermediate impurities of obeticholic acid were synthesized by using the readily available intermediate 5 as raw material.namely 6-β-ethyl-7-ketolithocholic acid(A),6-β-ethyl-7-keto-lithocholic acid methyl ester(B),3-α-acetyl-6-β-ethyl-7-ketolithocholic acid(C),6-α-ethyl-7-keto-lithocholic acid methyl ester(D),3-α-acetyl-6-α-ethyl-7-keto-lithocholic acid(E),and their structures were confirmed by ^(1)H NMR,^(13)C NMR and HR-MS.The single crystal data elucidated its configuration(impurity A),further confirming the structure of the compound.
作者
魏霞
文小清
母慧聪
黄晴菲
张燕
王启卫
WEI Xia;WEN Xiao-qing;MU Hui-cong;HUANG Qing-fei;ZHANG Yan;WANG Qi-wei(Chengdu Institute of Organic Chemistry,Chinese Academy of Sciences, Chengdu 610041, China;Graduate University of Chinese Academy of Sciences, Beijing 100049, China;College of Science, Xihua University, Chengdu 610039, China)
出处
《合成化学》
CAS
2021年第9期753-758,共6页
Chinese Journal of Synthetic Chemistry
基金
四川省科技计划项目应用基础(2019YJ0013)。
关键词
奥贝胆酸
杂质
合成
中间体
单晶
obeticholic acid
impurity
synthesis
intermediate
single crystal
