HRID973543
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To the solution of 6.35 g (0.05 mole) of 5-amino-3-dimethylamino-1H-1,2,4-triazole, 2.5 ml of acetic acid and 12.5 ml of dimethylformamide, 9.4 g (0.05 mole) of ethyl 3-oxo-3,4,5,6-tetrahydro-2H-thiopyrane-2-carboxylate are added and the reaction mixture is boiled for 40 minutes. The precipitated product is filtered off from the hot solution, then washed with acetic acid and i-propanol and recrystallized from dimethylformamide. Thus 8.2 g (65.2%) of 2-dimethylamino-5,7,8,9-tetrahydrothiopyrano[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidine-5(10H)-one are obtained. M.p.: higher than 350° C.
WORKUP
后处理
- filtrationThe precipitated product is filtered off from the hot solution
- washwashed with acetic acid and i-propanol
- customrecrystallized from dimethylformamide