HRID1915573
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 is dissolved in 500 ml dichloromethane. 500 ml brine, 250 ml ammonia solution 25% w/w and 34.0 g zinc powder are added and the mixture is stirred at room temperature for 1 h. The reaction mixture is filtrated over kieselgur and is washed with dichloromethane and water. The organic phase is separated and the water phase is extracted with dichloromethane. The combined dichloromethane phase is dried over Na2SO4 and the solvent is evaporated. The crude product is purified by chromatography on silica gel (dichloromethane/ethyl acetate) to yield the desired compound.
WORKUP
后处理
- filtrationThe reaction mixture is filtrated over kieselgur
- washis washed with dichloromethane and water
- customThe organic phase is separated
- extractionthe water phase is extracted with dichloromethane
- dry with materialThe combined dichloromethane phase is dried over Na2SO4
- customthe solvent is evaporated
- customThe crude product is purified by chromatography on silica gel (dichloromethane/ethyl acetate)