HRID2223873

反应详情

EQUATION

反应方程式

HRID 2223873 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

To 2-bromo-4-methylpyridine (15.5 g) was added 4-amino-1-benzylpiperidine (68.5 g). The resulting solution was stirred at 180° C. for 9 hours and then at 150° C. for 6 hours. Ethyl acetate and water were then added to the solution followed by addition of saturated aqueous sodium bicarbonate solution. After separating liquid layers, the organic layer was washed with water and saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and then, concentrated under reduced pressure. The resulting residue was purified by chromatography [silica gel, ethyl acetate-methanol-aqueous ammonia (90:10:0.1)] to give the title compound (11.5 g).

WORKUP

后处理

  1. waitat 150° C. for 6 hours
  2. customAfter separating liquid layers
  3. washthe organic layer was washed with water and saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting residue was purified by chromatography [silica gel, ethyl acetate-methanol-aqueous ammonia (90:10:0.1)]