HRID973544
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
0.976 g (0.0075 mole) of 5-amino-3-methylthio-1H-1,2,4-triazole are dissolved in 6 ml of acetic acid, then 1.368 g (0.075 mole) of ethyl 3-oxo-3,4,5,6-tetrahydro-2H-thiopyrane-4-carboxylate are added and the reaction mixture is boiled for 30 minutes. The precipitated product is filtered off from the hot solution, washed with water and recrystallized from dimethylformamide. Thus 1.2 g (62.9%) of 2-methylthio-5,6,7,9-tetrahydrothiopyrano[3,4-d]-1,2,4-triazolo[1,5-a]pyrimidine-5(10H)-one are obtained which melt at 294°-297° C.
WORKUP
后处理
- filtrationThe precipitated product is filtered off from the hot solution
- washwashed with water
- customrecrystallized from dimethylformamide