HRID1372385

反应详情

EQUATION

反应方程式

HRID 1372385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a suspension of 2.67 g (70 mmol) of lithium aluminum hydride in 100 mL of tetrahydrofuran was added dropwise a solution of 13.84 g (59 mmol) of 3-(2,4-dimethyl-1H-pyrrol-3-yl)-1-morpholin-4-yl-propan-1-one in 50 mL of tetrahydrofuran. The reaction mixture was stirred at 80° C. for 1 hour and cooled in an ice bath. Ice cubes were slowly added to the mixture until no more gas was generated. A few drops of 2 N sodium hydroxide were added and the reaction mixture was stirred at room temperature for 30 min, extracted with ethyl acetate and the extract dried over anhydrous sodium sulfate and concentrated to give 10.37 g (79% yield) of 4-[3-(2,4-dimethyl-1H-pyrrol-3-yl)-propyl]-morpholine as a light brown oil which was used without further purification.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. additionIce cubes were slowly added to the mixture until no more gas
  3. stirringthe reaction mixture was stirred at room temperature for 30 min
  4. extractionextracted with ethyl acetate
  5. dry with materialthe extract dried over anhydrous sodium sulfate
  6. concentrationconcentrated