第 38 卷第 5 期Vol. 38 No. 5
2008 年 10 月Oct 2008

所属栏目:医药及中间体

N,N-二甲基甲酰胺二甲基缩醛制备工艺优化
潘 毅,陈 蔚,陶 勇 (天津药物研究院,天津 300193)
摘 要:改进了N,N-二甲基甲酰胺二甲基缩醛(DMFA)的制备工艺,优化合成条件为:n(甲醇钠)∶n硫酸二甲酯)=1.2∶1、-5~5℃滴加亚胺络合物2,滴加时间2 h,-5~5℃反应2 h。在此条件下,收率由40%~70%提高至76%~80%,产品含量98%。
关键词:N,N-二甲基甲酰胺二甲基缩醛;工艺优化;中间体
中图分类号:TQ224.4  文献标识码:A  文章编号:1009-9212(2008)05- 0025-02
Optimieation on Synthesis Technology of N,N-Dimethylformamide Dimethyl Acetal
PAN Yi,CHEN Wei,TAO Yong (Tianjin Institute of Pharmaceutical Research (TIPR),Tianjin 300193,China)
Abstract:The preparative method of N,N-dimethylformamide dimethyl acetal was improved and optimized for its industrialized production. The optimal conditions were obstained as following:the molar ratio of n-sodium methylate and dimethyl sulfate was 1.2∶1,the reaction temperature was -5~5℃,and the reaction time was 4 h. The yield increases from 40%~70% to 76%~80%,and purity of product was 98%.
Key words:N,N-dimethylformamide dimethyl acetal;optimieation on synthesis technology;intermediate
作者简介:潘 毅(1973-),男,天津人,助理研究员,主要从事药物合成研究。(E-mail:panyi1973@sina.com)
收稿日期: 2008-06-2