HRID1854543

反应详情

EQUATION

反应方程式

HRID 1854543 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

Add water (2.94 L) and sodium hydrogen carbonate (648.25 g, 7.64 mol) to methyl 2-bromo-D-phenylalaninate hydrochloride (580 g, 1.91 mol) in dichloromethane (9.86 L) at 10° C. in an appropriate vessel. After 5 minutes add methyl chloroformate (198.53 g, 2.10 mol) and stir the mixture at 20° C. After 3 hours add water (2.5 L) and separate the layers. Extract the aqueous with dichloromethane, dry the combined organic extracts over sodium sulfate and concentrate under reduced pressure to give the title compound (556 g, 1.74 mol). MS (m/z): 315.8 (M+1 (79Br)), 317.8 (M+1 (81Br)).

WORKUP

后处理

  1. customseparate the layers
  2. extractionExtract the aqueous with dichloromethane
  3. dry with materialdry the combined organic extracts over sodium sulfate
  4. concentrationconcentrate under reduced pressure