HRID1087874

反应详情

EQUATION

反应方程式

HRID 1087874 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

0.83 g of L-phenylalanine (5 mmoles) are dissolved in aqueous dioxan (1: 2, 12 ml) containing 1.4 ml of triethylamine (10 mmoles). The mixture is cooled to 0° C. and 2.05 g (5 mmoles of the preceding carbonate dissolved in 4 ml of dioxan added at one time. After two hours at 0° C., 20 ml of water are added, followed by extraction twice with 20 ml of ether. The aqueous phase is then acidified (pH 2-3) with 6 N HCl followed by extraction three times with 50 ml of ethyl acetate. This is followed by drying over MgSO4 and evaporation. The product obtained crystallizes from ethyl acetate and petroleum-ether, and 1.44 g of the desired derivative obtained (yield 75%).

WORKUP

后处理

  1. additionadded at one time
  2. extractionfollowed by extraction twice with 20 ml of ether
  3. extractionfollowed by extraction three times with 50 ml of ethyl acetate
  4. dry with materialby drying over MgSO4 and evaporation
  5. customThe product obtained
  6. customcrystallizes from ethyl acetate and petroleum-ether, and 1.44 g of the desired derivative
  7. customobtained (yield 75%)