HRID1804552

反应详情

EQUATION

反应方程式

HRID 1804552 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

23.20 g (103.93 mmol) 3-benzyloxycarbonylamino-propionic acid, 14.10 g (104.35 mmol) 1-hydroxybenzotriazole, 18.80 ml (135.07 mmol) triethylamine and 21.00 g (135.27 mmol) (ethyl-3-(3-dimethylamino)-propylcarbondiimide hydrochloride (EDAC) are placed in 150 ml dichloromethane, cooled to 0° C. and stirred for 0.75 hours at this temperature. Then 10.50 g (114.26 mmol) 1-amino-2-butanol are added, the mixture is stirred for 2.5 hours at 0°-5° C. The reaction mixture is extracted with water and 1 molar sodium carbonate solution, the organic phase is dried and evaporated to dryness. The residue is extracted again with dichloromethane and sodium carbonate solution.

WORKUP

后处理

  1. stirringthe mixture is stirred for 2.5 hours at 0°-5° C
  2. extractionThe reaction mixture is extracted with water and 1 molar sodium carbonate solution
  3. customthe organic phase is dried
  4. customevaporated to dryness
  5. extractionThe residue is extracted again with dichloromethane and sodium carbonate solution