HRID1851158

反应详情

EQUATION

反应方程式

HRID 1851158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. filtrationThe reaction mixture was filtered through Celite
  2. washwas washed with dichloromethane and water
  3. customThe organic phase was separated
  4. extractionthe water phase was extracted with dichloromethane
  5. dry with materialThe combined dichloromethane phase was dried over Na2SO4
  6. customthe solvent was evaporated
  7. customThe crude product was purified by chromatography on silica gel (dichloromethane/ethyl acetate)