HRID1851158
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
34.5 g 5,7-dichloro-2-methyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine was dissolved in 500 mL dichloromethane. 500 mL brine, 250 mL 25% aqueous ammonia solution and 34.0 g zinc powder were added and the mixture was stirred at room temperature for 1 h. The reaction mixture was filtered through Celite and was washed with dichloromethane and water. The organic phase was separated and the water phase was extracted with dichloromethane. The combined dichloromethane phase was dried over Na2SO4 and the solvent was evaporated. The crude product was purified by chromatography on silica gel (dichloromethane/ethyl acetate) to yield the desired compound.
WORKUP
后处理
- filtrationThe reaction mixture was filtered through Celite
- washwas washed with dichloromethane and water
- customThe organic phase was separated
- extractionthe water phase was extracted with dichloromethane
- dry with materialThe combined dichloromethane phase was dried over Na2SO4
- customthe solvent was evaporated
- customThe crude product was purified by chromatography on silica gel (dichloromethane/ethyl acetate)