摘要
以2-氯-1,3-二(2,4,6-三甲基苯基)咪唑盐酸盐(IMesCl-Cl)作缩合剂,熊(鹅)去氧胆酸为原料,直接与甘氨酸乙酯盐酸盐反应,采用一锅法制得关键中间体甘氨熊(鹅)去氧胆酸乙酯2a和2b;2a和2b在碱性条件下水解合成了甘氨熊(鹅)去氧胆酸3a和3b,总收率超过83%,其结构经^(1)H NMR,^(13)C NMR和HR-MS(ESI)确证。
The key intermediate,ethyl glycoursodeoxycholic acid ethyl ester(2a)and glycourchenodeoxycholic acid ethyl ester(2b),were synthesized from ursodeoxycholic acid and chenodeoxycholic acid and glycine ethyl ester hydrochloride by employing IMesCl-Cl as a condensation reagent.Then glycoursodeoxycholic acid(3a)and glycourchenodeoxycholic acid(3b)were obtained by hydrolysis reaction of 2a and 2b under alkaline condition with total yield up to 83%.The structures were confirmed by ^(1)H NMR,^(13)C NMR and HR-MS(ESI).
作者
魏霞
韩洁
陈娟
李长任
黄晴菲
张燕
王启卫
WEI Xia;HAN Jie;CHEN Juan;LI Chang-ren;HUANG Qing-fei;ZHANG Yan;WANG Qi-wei(Chengdu Institute of Organic Chemistry, Chinese Academy of Sciences, Chengdu 610041, China;University of Chinese Academy of Sciences, Beijing 100049, China;Department of Chemistry, Xihua University, Chengdu 610039, China;College of Chemistry & Environmental Protection Engineering, Southwest Minzu University, Chengdu 610225, China)
出处
《合成化学》
CAS
2021年第8期705-709,共5页
Chinese Journal of Synthetic Chemistry
基金
四川省科技厅应用基础项目(2019YJ0013)。
