HRID627541

反应详情

EQUATION

反应方程式

HRID 627541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

n-BuLi (1.6 M in hexane, 79 mL, 126 mmol) was added dropwise to a mixture of hexamethyldisilazane (26.7 mL, 126 mmol) in THF (150 mL) at −78° C. under nitrogen. The mixture was stirred for 1 hour, then was warmed to −40° C. A solution of methyl 5-bromo-2-(2-(3-chlorophenyl)acetamido)benzoate (21.1 g, 55 mmol, Intermediate 60, step a) in THF (150 mL) was added. The mixture was allowed to warm to room temperature and ice was added. The aqueous phase was acidified with 6 N aqueous HCl. The precipitate was collected by filtration, washed with DCM, and air-dried to yield the title compound.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. additionice was added
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with DCM
  5. customair-dried