三乙胺催化合成2,5-二巯基-1,3,4-噻二唑

Synthesis of 2,5-Dimercapto-1,3,4-thiadiazole Using Triethylamine as Catalyst

采用三乙胺作为催化剂,合成了DMTD(2,5-二巯基-1,3,4-噻二唑),将产率从传统工艺的82.50％提高至90.01％,并探讨了三乙胺的催化机理。通过试验得到了该反应的最佳反应条件:反应温度为80℃;配料比为n(水合肼):n(二硫化碳):n(氢氧化钾)=10:3.5:2.0;每摩尔水合肼需加三乙胺40mg。同时用红外光谱仪鉴定了产物的结构,并进行了氮元素的分析及熔点的测定,结果均与理论值相符。

2,5-Dimercapto-1,3,4-thiadiazole was prepared by using triethylamine as the catalyst. Compared with traditional synthesis techniques, the reaction yields were from 82.50% to 90.01% greater if triethylamine was used as the catalyst. The mechanism of catalysis was studied and the optimal reaction conditions were found by experiments. The optimum mole ratios were: hydrazine hydrate: carbon disulflde: KOH= 1.0: 3.5: 2.0, the reaction temperature 80℃ and 40 mg triethylamine was required. The structure of the product was identified by infrared spectra, the nitrogen content and melting point of the product were determined. The results conformed to the theoretical values.