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[目的]探讨不同操作方法、水合肼用量、反应时间、反应温度等条件对反应收率的影响,对合成工艺进行优化研究。[方法]以二硫化碳、甲胺、三乙胺、水合肼为原料反应得到4-甲基氨基硫脲。[结果]粗品经重结晶后得到白色固体4-甲基氨基硫脲,收率为82.9%。采用UV、IR、~1H NMR表征了产物的分子结构。[结论]确定最佳的工艺条件为二硫化碳、甲胺、三乙胺、水合肼摩尔比为1:1:1:1.2,在100℃下反应2 h,放大实验中,产品收率略有提高。
[Objective] The research aimed to discuss the influence of different operation methods, hydrazine hydrate dosage, reaction time and reaction temperature on the yield of the reaction, and optimize the synthesis process. [Method] Carbon disulfide, methylamine, triethylamine and hydrazine hydrate were used as raw materials to get 4 - methylthiosemicarbazone. [Result] The crude product was recrystallized to obtain white solid 4-methylthiosemicarbazone in a yield of 82.9%. The molecular structure of the product was characterized by UV, IR and 1H NMR. [Conclusion] The optimum process conditions were as follows: the molar ratio of carbon disulfide, methylamine, triethylamine and hydrazine hydrate was 1: 1: 1: 1.2. After reaction at 100 ℃ for 2 h, the product yield increased slightly .