N′-烷基-N, N-二甲基乙脒基碳酸氢盐制备及其表征.docVIP

N′-烷基-N,N-二甲基乙脒基碳酸氢盐 程云，叶志文＊ （南京理工大学化工学院 江苏 南京 210094） 摘要：以烷基胺N,N-二甲基乙酰胺DMAC）和硫酸二甲酯为原料， N′-烷基-N,N-二甲基乙脒，与过量干冰反应目标产物N′-烷基-N,N-二甲基乙脒基碳酸氢盐N′-十二烷基-N,N-二甲基乙脒POCl3为脱水剂和PH调节剂，原料投料比为n（）：n（DMAC）：n（POCl3）=12.5：0.3565～70℃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））=1.2：1，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IR、MS1HNMR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 five compounds 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)=1:2.5:0.35, 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-dimethylacetamidinium bicarbonates. What’s more, better technology of intermediate product N’-alkyl-N,N-dimethylacetamidine was probed, with the yield increasing 18% compared with the reported, and the optional conditions were as follows: n(sodium methoxide):n(dimethyl sulfite)=1.2:1, the time of adding imine-complex is controlled within 2 hours under 0℃，and the reaction time is controlled around 3 hours under -5℃. Infrared Spectroscopy(IR), Mass Spectra(MS) and 1H Nuclear Magnetic Resonance(1HNMR) were used to confirm the structure of N’-alkyl-N,N-dimethylacetamidinium bicarbonates. Keywords: Amidine; Switchable; Surfactant; Synthesis; 1引言 在诸如石油开采，原油回收，食品加工，乳液聚合等化学工业过程中，表面活性剂的应用十分广泛，它能起到稳定液-液或气-液界面，增溶疏水有机