N′-烷基-N, N-二甲基乙脒基碳酸氢盐的制备及其表征.doc

文档介绍：N′-烷基-N,N-二甲基乙脒基碳酸氢盐的制备及其表征
程云,叶志文*
(南京理工大学化工学院江苏南京 210094)
摘要:以系列烷基胺、N,N-二甲基乙酰胺(DMAC)和硫酸二甲酯为原料,采用直接法制备五个系列中间产物 N′-烷基-N,N-二甲基乙脒,并与过量干冰反应合成系列目标产物N′-烷基-N,N-二甲基乙脒基碳酸氢盐。本文对合成N′-十二烷基-N,N-二甲基乙脒的工艺条件进行了优化,确定其最佳反应条件为:以氯仿为溶剂,POCl3为脱水剂和PH调节剂,原料投料比为n(十二胺):n(DMAC):n(POCl3)=1::,于65~70℃下反应24h,产率大于85%。采用间接法制备中间产物N,N-二甲基乙酰胺二甲基缩醛,并对其工艺条件进行优化,确定最佳反应条件为:原料投料比(n(甲醇钠):n(硫酸二甲酯))=:1,在0℃下控制滴加亚胺络合物时间为2h,并在-5℃下反应3h,产率达到47%。以N′-十二烷基-N,N-二甲基乙脒基碳酸氢盐为例,通过IR、MS和1HNMR等分析手段对产物进行了表征。
关键词:脒基;开关型;表面活性剂;合成
The synthesis of N′-alkyl-N,N-dimethylacetamidinium
bicarbonates and it’s characterization
Cheng Yun, Ye Zhi-wen*
(College of Chemical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China)
Abstract:Alkylamines, N,N-dimethylacetamide and dimethyl sulfate were used to synthesize pounds of N’-alkyl-N,N-dimethylacetamidine through the direct method. Then the target products, N’-alkyl-N,N-dimethylacetamidinium bicarbonates, were obtained by reacting with a large number of dry ice. The optional conditions of direct method of synthesizing N’-dodecyl-N,N-dimethylacetamidine were studied as follows: POCl3 as catalyst, chloroform as solvent, n(dodecylamine):n(DMAC):n(POCl3)=1::, 65~70℃ for 24h. The yield of the product was above 85%.The intermediate product N’-alkyl-N,N-dimethylacetamidine were synthesized through indirect method of preparing N’-alkyl-N,N-dimethylacetamid