化工中间体三嗪环产业化工艺研究
Study on Industrialization Process of Thiotriazinone
于永宏 1林琳1
作者信息
- 1. 辽宁美亚制药有限公司, 辽宁 抚顺 113122
- 折叠
摘要
目的:通过找出最佳工艺条件,提高产品质量和收率,利于产业化生产控制.方法:在混合溶剂中(一种极性质子溶剂和一种极性非质子溶剂)中,2-甲氨基硫脲、草酸二乙酯、甲醇钠在0～45℃缩合生成三嗪钠,然后经盐酸酸化得到目标产物三嗪环(TTZ).结果:通过混合溶剂的使用,合成过程体系黏稠度得到大幅度改善,三嗪环(TTZ)收率提高到90%以上(以2-甲氨基硫脲计),纯度平均在99.5%以上,副产物1-甲基-5-巯基-1,2,4-三氮唑-3-羧酸甲酯(TTA)在0.1%以下.结论:该方法是合成三嗪环(TTZ)适宜的工业化方法.
Abstract
In order to improve the product quality and yield by finding out the optimal technological conditions,thiotriazinone sodium was synthesized by condensation of 2-methyl-3-thiosemicarbazide,diethyl oxalate and sodium methylate in a mixed solvent(a polar proton solvent and a polar non-proton solvent)at 0～45℃,then the target product thiotriazinone(TTZ)was obtained by hydrochloric acid acidification.By using mixed solvents,the viscosity of the synthesized process system was greatly improved,the yield of thiotriazinone(TTZ)was increased to more than 90%(calculated by 2-methyl-3-thiosemicarbazide),and the average purity was over 99.5%,the by-product material,1-methyl-5-mercapto-1,2,4-triazole-3-carboxylate(TTA),was less than 0.1%.So,this industrial method is suitable for the synthesis of thiotriazinone(TTZ).
关键词
中间体/三嗪环(TTZ)/合成/方法Key words
Intermediate/Thiotriazinone(TTZ)/Synthesis/Method引用本文复制引用
出版年
2024
NETL
NSTL
万方数据