HRID1836992

反应详情

EQUATION

反应方程式

HRID 1836992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of crude (5-methyl-1H-imidazol-4-yl)methyl[4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidin-2yl]formamide (0.27 g, 0.615 mmol) in ethanol (10 ml) and 2N hydrochloric acid (10 ml) was heated under reflux for 2 h. The solvents were then evaporated and the residue basified with 0.880 ammonia and extracted with DCM. The dried organic phase was evaporated onto silica gel and this mixture was purified on a silica gel SPE cartridge. Elution with DCM:ethanol:0.880 ammonia, 91:8:1, gave the title compound as a colourless crystalline solid (0.14 g).

WORKUP

后处理

  1. temperatureunder reflux for 2 h
  2. customThe solvents were then evaporated
  3. extractionextracted with DCM
  4. customThe dried organic phase was evaporated onto silica gel
  5. customthis mixture was purified on a silica gel SPE cartridge
  6. washElution with DCM