微纳米碳酸钾法合成N-甲基-1-甲硫基-2-硝基乙烯胺  

Synthesis of N-methyl-1-methylthio-2-nitroethenamine via Macronano-K_2CO_3

作　　者：李军章[1,2,3] 王家喜[2] 

机构地区：[1]河北工业大学化工学院,天津030013 [2]河北科技大学化学与制药工程学院,河北石家庄050018 [3]河北省药物化工工程技术研究中心,河北石家庄050018

出　　处：《河北师范大学学报（自然科学版）》2012年第5期485-488,508,共5页Journal of Hebei Normal University：Natural Science

基　　金：国家自然科学基金(30873139);河北省自然科学基金(10276406D)

摘　　要：在高频共振研磨机中采用湿法研磨制备了微纳米K2CO3,比表面积1.69m2/g,平均粒径266nm.以微纳米K2CO3为碱,硝基甲烷和异硫氰酸甲酯在无水乙醇中反应得到1-甲胺基-2-硝基乙烯硫醇钾(单钾盐),避免了传统工艺中异硫氰酸甲酯与强碱的副反应,单钾盐收率高;然后在水溶液中与硫酸二甲酯反应得到N-甲基-1-甲硫基-2-硝基乙烯胺,避免了有毒有机溶剂的使用,工艺过程更环保.探讨了微纳米K2CO3对第1步反应及反应温度对第2步反应的影响,优化后2步反应总收率为86%.通过FTIR和1 HNMR表征了化合物的结构.Macronano-K2CO3 particles with mean size of 266 nm and specific surface area of 1.69 m2/g were prepared via wet milling method for 5 h through a resonance mill.Using macronano-K2CO3 as base,potassium salt 1-methylamino-2-nitroethenethiolate（monopotassium salt） was synthesized from nitromethane and methyl isothiocyanate in anhydrous EtOH,the yield of monopotassium salt was very high because the side reaction was avoided caused by methyl isothiocynate reacting with strong base;and then it reacted with dimethyl sulfate in water to give N-methyl-1-methylthio-2-nitroethenamine,the process was more environmentally friendly toxic because harmful organic solvent was not used.The effects of macronano-K2CO3 on the first step reaction and reaction temperature on the second step reaction were investigated.The optimized overall yield was 86 %.The target product was characterized by means of FTIR and1HNMR.

关 键 词：N-甲基-1-甲硫基-2-硝基乙烯胺 微纳米K2CO3 异硫氰酸甲酯 

分 类 号：O622.7[理学—有机化学]