第 38 卷第 5 期 |  | Vol. 38 No. 5 | 2008 年 10 月 | Oct 2008 |
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所屬欄目:醫藥及中間體
N,N-二甲基甲酰胺二甲基縮醛制備工藝優(yōu)化 |
潘 毅,陳 蔚,陶 勇
(天津藥物研究院,天津 300193) |
摘 要:改進(jìn)了N,N-二甲基甲酰胺二甲基縮醛(DMFA)的制備工藝,優(yōu)化合成條件為:n(甲醇鈉)∶n硫酸二甲酯)=1.2∶1、-5~5℃滴加亞胺絡(luò )合物2,滴加時(shí)間2 h,-5~5℃反應2 h。在此條件下,收率由40%~70%提高至76%~80%,產(chǎn)品含量98%。 |
關(guān)鍵詞:N,N-二甲基甲酰胺二甲基縮醛;工藝優(yōu)化;中間體 |
中圖分類(lèi)號:TQ224.4 文獻標識碼:A 文章編號:1009-9212(2008)05- 0025-02 |
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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 |
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作者簡(jiǎn)介:潘 毅(1973-),男,天津人,助理研究員,主要從事藥物合成研究。(E-mail:panyi1973@sina.com)
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收稿日期: 2008-06-2
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