HRID515154

反应详情

EQUATION

反应方程式

HRID 515154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

4-Chloro-2-(ethylsulfonyl)-6-methyl-benzonitrile (0.43 g, 1.77 mmol), morpholine (0.46 ml, 5.31 mmol) and potassium carbonate (0.32 g, 2.30 mmol) are taken up in N-methyl-2-pyrrolidone (3 ml) in a sealed tube and the resulting mixture is heated at 150° C. for 2 d. The mixture is then diluted with water (6 ml) and extracted with ethyl acetate (3×10 ml). The organic layer is washed with water (2×10 ml), brine (20 ml), dried over anhydrous sodium sulfate and evaporated to get the crude product, which is purified by column chromatography (silica gel, 25% ethyl acetate/hexane) to yield 2-(ethylsulfonyl)-6-methyl-4-morpholin-4-yl-benzonitrile (0.50 g, 1.70 mmol, 96%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×10 ml)
  2. washThe organic layer is washed with water (2×10 ml), brine (20 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated
  5. customto get the crude product, which
  6. customis purified by column chromatography (silica gel, 25% ethyl acetate/hexane)