微波促进合成六亚甲基-1,6-二氨基甲酸甲酯的研究  

Synthesis of Dimethylhexane-1,6-Dicarbamate under Microwave Irradiation

作　　者：郑志花[1] 王建龙[1] 陈丽珍[1] 

机构地区：[1]中北大学化工与环境学院,山西太原030051

出　　处：《中北大学学报（自然科学版）》2014年第4期438-443,共6页Journal of North University of China(Natural Science Edition)

基　　金：中北大学科学基金项目

摘　　要：研究了常压下微波加热促进碳酸二甲酯与1,6-己二胺合成六亚甲基-1,6-二氨基甲酸甲酯的反应,考察了有无催化剂、催化剂种类及用量、原料配比及反应温度、反应时间对六亚甲基-1,6-二氨基甲酸甲酯得率的影响.实验结果表明,微波对此反应有很好的促进作用,不仅使产品得率提高,而且可大大缩短反应时间.获得的较佳工艺条件为:1,6-己二胺与碳酸二甲酯的物质的量的比为4:1时,四乙基溴化铵为催化剂,加入量为1,6-己二胺物质的量的0.3%,85℃下,反应30 min,经稀盐酸洗涤,乙醇重结晶,制得六亚甲基-1,6-二氨基甲酸甲酯,平均得率为82.0%.同时对产物进行了红外光谱、核磁共振氢谱及元素分析表征.Dimethylhexane-1, 6-dicarbamate was synthesized by microwave heating under atmospheric pres- sure with dimethyl carbonate and hexane-1, 6-diamine. The influencing factors on yield of dimethylhexane-1, 6-dicarbamate were investigated, such as the presence of catalyst, the kind and amount of catalyst, raw mate- rial ratio, reaction temperature and reaction time. The experimental results show that microwave reaction has a good promoting effect, not only in improving the product yield greatly in shortening the reaction time. The better process conditions are organized as follows： the ratio of hexane-1, 6-diamine and dimethyl carbonate is 4 ： 1, tetraethyl ammonium bromide is used as catalyst and addition amount of hexane-I, 6-diamine is 0.3 %, at 85℃ and after reacting 30 min, through washing with the dilute hydrochloric acid and recrystallization with ethanol, dimethylhexane-1, 6-dicarhamate gets average yield of 82%. The structure of production is characterized by FT-IR, 1HNMR and elemental analysis.

关 键 词：碳酸二甲酯 1 6-己二胺 六亚甲基-1 6-二氨基甲酸甲酯 微波加热 

分 类 号：TQ225.52[化学工程—有机化工] TQ226.36