Study on Industrialization Process of Thiotriazinone
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).
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