HRID2120241

反应详情

EQUATION

反应方程式

HRID 2120241 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 the suspension of lithium aluminum hydride (2.3 g, 60 mmol) in tetrahydrofuran (50 mL) was added a solution of 3-(2,4-dimethyl-1H-pyrrol-3-yl)-N,N-dimethyl-propionamide (9.81 g, 50 mmol) in THF (50 mL) dropwise. The reaction mixture was stirred at 80° C. for 1 hour and cooled with ice bath. Ice cube was added into the reaction mixture slowly until no more gas generated. A few drops of 2 N sodium hydroxide was added and the reaction mixture was stirred at room temperature for 30 minutes, extracted with ethyl acetate, dried over anhydrous sodium sulfate and concentrated to give 6.8 g (75%) of [3-(2,4-dimethyl-1H-pyrrol-3-yl)-propyl]-dimethylamine as an orange oil which was used without further purification.

WORKUP

后处理

  1. temperaturecooled with ice bath
  2. additionIce cube was added into the reaction mixture slowly until no more gas
  3. stirringthe reaction mixture was stirred at room temperature for 30 minutes
  4. extractionextracted with ethyl acetate
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated