HRID1076424

反应详情

EQUATION

反应方程式

HRID 1076424 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

5.27 g of Z-Thr(tBu)-OH and 1.56 g of H-Pro-NH2 are dissolved in 60 ml of acetonitrile, the solution is cooled to 0°C and 3.11 g of dicyclohexylcarbodiimide are added. After 1 hour at 0°C and 20 hours at room temperature the dicyclohexylurea is filtered off and the filtrate is evaporated and the residue taken up in ethyl acetate. The ethyl acetate solution is washed with dilute citric acid solution, soda solution and water, and is dried with sodium sulphate and evaporated. On thin layer chromatography on silica gel plates the colourless residue shows Rf45 = 0.76; Rf43c = 0.70; Rf52 = 0.62.

WORKUP

后处理

  1. filtration20 hours at room temperature the dicyclohexylurea is filtered off
  2. customthe filtrate is evaporated
  3. washThe ethyl acetate solution is washed with dilute citric acid solution, soda solution and water
  4. dry with materialis dried with sodium sulphate
  5. customevaporated