反应详情

1.5 ml (13 mmole) of Et3N, 1.38 g of 5-chlorovaleroyl chloride and 80 ml of 4-DMAP are successively added to 2 g of 5-amino-2-benzylmercapto-1,3,4-thiadiazole (8.9 mmole) suspended in 5 ml of anhydrous methylene chloride at room temperature with stirring and under nitrogen atmosphere. The reaction is checked by TLC (10% methanol in chloroform) and it is complete after 3 hours. The solid product so formed is filtered, washed with water and purified by crystallization from ethanol. 2.7 g of 5-chlorovaleroylamino-2-benzylmercapto-1,3,4-thiadiazole is obtained with melting point 145°-148° C. and 90% yield.

1. customThe solid product so formed
2. filtrationis filtered
3. washwashed with water
4. custompurified by crystallization from ethanol