【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。更多还原

【Abstract】 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-1-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 FTIR and 1HNMR.更多还原