摘要
手性控制是药物研究的重要组成部分。以保持手性骨架的碳环糖为原料,与2-氨基-6-苄氧基嘌呤缩合后,经过氨基保护、Dess-Martin氧化、亚甲基化、脱保护等6步反应,制得恩替卡韦对映异构体,总得率37%。通过二维核磁NOESY实验确定对映异构体绝对构型后,建立恩替卡韦与其对映异构体的HPLC分析方法,用于恩替卡韦原料药的手性质量控制。
Chiral contlol was an important constitute in pharmaceutical study. This article reports a synthetic method of enantiomer of entecavir, which was prepared via 6 steps including condensation, amino protection, Dess-Martin oxidation, methylene and deprotection from carbocyclic sugar with corresponding chiral skeleton and 2-amino-6-benzyloxy purine as materials, with total yield 37%. HPLC analysis method was estanlishod to be applied in chiral control for entecavir API after determination for absolute configuration of enantiomer by 2D NOESY NMR.
出处
《化学研究与应用》
CAS
CSCD
北大核心
2012年第12期1814-1818,共5页
Chemical Research and Application
基金
安徽省自然科学基金项目(1208085QB23)资助
