HRID991591

反应详情

EQUATION

反应方程式

HRID 991591 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

4-amino-2-methylbenzimidazole (0.6 g, 4,1 mmol) was dissolved in acetonitrile (10 ml). To the solution were added 2,6-dimethyl-4-fluoro-benzylbenzylbromide (0.89 g, 4,1 mol) and potassium carbonate (0.68 g, 4.9 mmol) and the mixture was warmed at 70-80° C. for 3 h. The reaction mixture was cooled to room temperature and methylene chloride (25 ml) and water (25 ml) was added. The organic layer was separated, dried over sodium sulfate and was evaporated under reduced pressure. The residue was crystallized twice from ethyl acetate and was purified by column chromatography on silica gel, using methylene chloride containing 10% methanol as eluent. There was obtained 0.26 g (22%) of the title compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customThe organic layer was separated
  3. dry with materialdried over sodium sulfate
  4. customwas evaporated under reduced pressure
  5. customThe residue was crystallized twice from ethyl acetate
  6. customwas purified by column chromatography on silica gel