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米非司酮衍生物制备中格氏反应副产物的结构鉴定
引用本文:陈安平,雷小平.米非司酮衍生物制备中格氏反应副产物的结构鉴定[J].中国药学,2004,13(1):19-23.
作者姓名:陈安平  雷小平
作者单位:北京大学药学院药物化学系 100083 (陈安平),北京大学药学院药物化学系 100083(雷小平)
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  米非司酮衍生物  二维光谱分析

Structure Determination of By-product in Grignard Reaction for Preparing Mifepristone Derivatives
CHEN An-ping,LEI Xiao-ping.Structure Determination of By-product in Grignard Reaction for Preparing Mifepristone Derivatives[J].Journal of Chinese Pharmaceutical Sciences,2004,13(1):19-23.
Authors:CHEN An-ping  LEI Xiao-ping
Abstract:AimTo determine the structure of the by-pro du ct produced in Grignard reaction for preparing mifepristone derivatives, and elu cidate the reaction mechanism. MethodsThe structure of t he by-product was determined with elemental analysis, one- and two-dimension spectra NMR (DEPT, 1H- 1Hcosy, HMQC, HMBC) and compared with those o f mifepristone. ResultsThe main by-product was 11,17-d i-addition product of Grignard reagent of N, N-dimethylamino phenyl bromide. ConclusionThis is the first complete assignment of 1H NMR and 13 C NMR of compound (3).
Keywords:by-product identification  mifepristone derivatives  two-dimension NMR
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