http://jcps.bjmu.edu.cn

• 研究论文 • 上一篇    下一篇

米非司酮衍生物制备中格氏反应副产物的结构鉴定

陈安平, 雷小平*   

  1. 北京大学药学院药物化学系, 100083
  • 收稿日期:2003-10-05 修回日期:2004-02-10 出版日期:2004-03-15 发布日期:2004-03-15
  • 通讯作者: 雷小平*

Structure Determination of By-product in Grignard Reaction for Preparing Mifepristone Derivatives

CHEN An-ping, LEI Xiao-ping*   

  1. Department of Medicinal Chemistry, School of Pharmaceutical Sciences,Peking Uni versity, Beijing 100083, China
  • Received:2003-10-05 Revised:2004-02-10 Online:2004-03-15 Published:2004-03-15
  • Contact: LEI Xiao-ping*

摘要: 目的 确定米非司酮衍生物制备过程中格氏反应一步的副产物的结构, 并分析反应机理. 方法 通过一维及二维光谱分析和元素分析确定副产物的结构. 结果 证实了副产物是11,17位双加成的格氏反应的产物. 结论 这是首次对此步副产物用光谱进行C, H的详细归属.

关键词: 副产物结构鉴定, 副产物结构鉴定, 米非司酮衍生物, 米非司酮衍生物, 二维光谱分析, 二维光谱分析

Abstract: Aim To determine the structure of the by-product produced in Grignard reaction for preparing mifepristone derivatives, and elucidate the reaction mechanism. Methods The structure of the by-product was determined with elemental analysis, one- and two-dimension spectra NMR (DEPT, 1H-1Hcosy, HMQC, HMBC) and compared with those of mifepristone. Results The main by-product was 11,17-di-addition product of Grignard reagent of N, N-dimethylamino phenyl bromide. Conclusion This is the first complete assignment of 1H NMR and 13C NMR of compound (3).

Key words: by-product identification, by-product identification, mifepristone deriva tives, mifepristone deriva tives, two-dimension NMR, two-dimension NMR

中图分类号: 

Supporting: *Corresponding author. Tel.: 010-82801505