1-甲胺基-1-甲硫基-2-硝基乙烯的合成  

Synthesis of 1-Methylamino-1-methylthio-2-nitroethylene

作　　者：李军章[1,2,3] 王家喜[1] 刘守信[2,3] 

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050071 [3]河北省药物化工工程技术研究中心,河北石家庄050071

出　　处：《精细化工》2012年第8期787-789,794,共4页Fine Chemicals

摘　　要：在高频共振研磨机中采用湿法研磨5 h制备了平均粒径为266 nm的微纳米碳酸钾。以微纳米碳酸钾为碱,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,然后在水溶液中与硫酸二甲酯反应得到1-甲胺基-1-甲硫基-2-硝基乙烯。探讨了物料比、反应温度、反应时间对第1步反应的影响,优化后两步反应总收率为86%。化合物的结构通过FTIR和1HNMR进行了表征。Macronano-K2CO3 of a particle size of 266 nm was prepared via wet milling method for 5 h through resonance mill. Using macronano-K2CO3 as base, potassium 1-methylamino-2- nitroethylenethiolate was synthesized from nitromethane and methyl isothiocyanate in anhydrous EtOH, and then reacted with dimethyl sulfate in water to give 1-methylamino-l-methylthio-2-nitroethylene. The effects of molar ratio of raw materials, reaction temperature and reaction time on the first-step reaction were investigated. The optimized overall yield was 86%. The target product was characterized by means of FFIR and 1HNMR.

关 键 词：1-甲胺基-1-甲硫基-2-硝基乙烯 微纳米碳酸钾 异硫氰酸甲酯 医药与日化原料 

分 类 号：TQ460.31[化学工程—制药化工]