一种N,N-二甲基甲酰胺二甲缩醛的温和合成方法  

Mild Synthesis Method of N,N-Dimethylformamide Dimethylacetal

作　　者：刘玉霞[1,2] 王有为 柴勇利[1,2] 崔炳春[1,2] 刘菲[1,2] LIU Yuxia;WANG Youwei;CHAI Yongli;CUI Bingchun;LIU Fei(Henan Chemical Industry Research Institute Co. Ltd.,Zhengzhou 450052,China;Henan Key Laboratory of Chemical Catalysis,Zhengzhou 450052,China;Henan Kai Xiang Fine Chemical Co. Ltd.,Sanmenxia 472300,Henan China)

机构地区：[1]河南省化工研究所有限责任公司,郑州450052 [2]河南省化学催化重点实验室,郑州450052 [3]河南开祥精细化工有限公司,河南三门峡472300

出　　处：《河南科学》2017年第2期196-199,共4页Henan Science

基　　金：河南省科技攻关项目(162102210138)

摘　　要：选用新的有机溶剂获得一种N,N-二甲基甲酰胺二甲缩醛(DMFDMA)的温和合成方法,以异构烷烃作为合成DMFDMA的一种新型有机溶剂,考察了反应温度、有机溶剂种类、原料配比、反应时间对产品收率的影响.优化的工艺条件为:第一步反应温度为75℃、异构烷烃作为有机溶剂、n(甲醇钠)∶n(亚胺络合物)=1.2∶1、第二步反应时间是滴加2 h和反应2 h.该条件下,DMFDMA收率达到85.41%,粗产品纯度为97%.采用红外光谱(IR)、核磁分析仪(NMR)、液相色谱-质谱联用仪(LC-MS)对样品进行表征.该合成工艺收率高,操作简单,条件温和,适合工业化生产.N,N-Dimethylformamide dimethylacetal was synthesized successfully by the mild method,this paper used the isoparaffin as a new type of organic solvent. The effect of the reaction temperature,organic solvent type,the mole ratio of substrates and time of reaction on yield of the product were investigated. The optimized experimental parameters were as follows:the reaction temperature was 75 ℃ in the first step reactions. We selected the isoparaffin as the organic solvent.The mole ratio of sodium methoxide and the amine complex compound was 1.2∶1. The drop and reaction time was 2 hrespectively. Under the optimized conditions,the yield of DMFDMA was 85.41% and the purity was 97%. The sample with the highest yield was characterized by the infrared spectroscopy,the nuclear magnetic resonance spectrum and the liquid chromatograph-mass spectrometer. The synthesis process was suitable for the industrial application with the advantages of high yield and easy to operate under the mild operation condition.

关 键 词：N N-二甲基甲酰胺二甲缩醛 异构烷烃 温和合成方法 医药中间体 

分 类 号：O623.541[理学—有机化学] TQ224.4[理学—化学]