HRID53165

反应详情

EQUATION

反应方程式

HRID 53165 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Pyrrolo[2,3-b]pyridine (2.00 g, 16.93 mmol) is dissolved in dimethylformamide (15.0 ml) under an argon atmosphere. Sodium hydride (60% in oil) (0.96 g, 40.0 mmol, 1.5 equiv.) is added at 0° C. over a period of 30 minutes. After 30 minutes' stirring at 0° C., iodomethane (1.49 ml, 24.02 mmol, 1.5 equiv.) is added dropwise. After returning to room temperature, the reaction mixture is stirred for 1 hour. The dimethylformamide is evaporated off under reduced pressure, and the product is taken up in water and extracted with dichloromethane. Purification on a silica column (petroleum ether/ethyl acetate 7/3) allows isolation of the title compound in the form of an oil in a yield of 99%. ##STR31##

WORKUP

后处理

  1. customAfter returning to room temperature
  2. stirringthe reaction mixture is stirred for 1 hour
  3. customThe dimethylformamide is evaporated off under reduced pressure
  4. extractionextracted with dichloromethane
  5. customPurification on a silica column (petroleum ether/ethyl acetate 7/3)