HRID1525919

反应详情

EQUATION

反应方程式

HRID 1525919 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 2-(4-bromo-2,6-difluorophenyl)acetamide (0.4 g, 1.6 mmol) in carbon tetrachloride (5 mL) was degassed with nitrogen for 5 min. To this was added N-bromosuccinimide (0.28 g, 1.6 mmol) and then azobisisobutyronitrile (0.039 g, 0.24 mmol) while stirring. The reaction mixture was stirred at 80° C. overnight and then cooled to room temperature. The reaction mixture was concentrated to dryness in vacuo, and the residue was purified by flash chromatography (0-100% ethyl acetate/hexanes) to afford the title product (60 mg, 11%). MS(ES)+ m/e 328 [M+H]+.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. concentrationThe reaction mixture was concentrated to dryness in vacuo
  3. customthe residue was purified by flash chromatography (0-100% ethyl acetate/hexanes)