HRID7548

反应详情

EQUATION

反应方程式

HRID 7548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

35 g (339 mmol) 2-aminobutanoic acid and 75.6 g (747 mmol) triethylamine are suspended in 300 ml of dichloromethane and stirred at 0° C. 81 g (747 mmol) chlorotrimethylsilane are added dropwise, then the mixture is stirred for 1 hour at room temperature and 1 hour at 40° C. After cooling down at −10° C., 45 g (339 mmol) cyclopentanecarbonyl chloride are added slowly. The reaction mixture is stirred for 2 hours at −10° C. and then 1 hour at room temperature. At 0° C., 50 ml of water are added. The mixture is diluted with water and dichloromethane, filtered and the solid product washed with water/dichloromethane 9/1, toluene and diethylether.

WORKUP

后处理

  1. stirringthe mixture is stirred for 1 hour at room temperature and 1 hour at 40° C
  2. temperatureAfter cooling down at −10° C.
  3. stirringThe reaction mixture is stirred for 2 hours at −10° C.
  4. custom1 hour
  5. customat room temperature
  6. filtrationfiltered
  7. washthe solid product washed with water/dichloromethane 9/1, toluene and diethylether