HRID333022

反应详情

EQUATION

反应方程式

HRID 333022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

3-Bromo-4-fluorobenzonitrile (10.0 g, 50 mmol, 1 eq) and imidazole (5.1 g, 75 mmol, 1.5 eq) are dissolved in dimethylformamide (100 ml) and carefully admixed with sodium hydride (60% in mineral oil, 3.0 g, 75 mmol, 1.5 eq) under nitrogen at room temperature. The mixture is stirred at 100° C. for 4 hours. After cooling to room temperature, water (10 ml) is added and the mixture is evaporated to dryness. The residue is washed with water and petroleum ether and purified by column chromatography (silica gel, methyl tert-butyl ether/ethyl acetate gradient).

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. customthe mixture is evaporated to dryness
  3. washThe residue is washed with water and petroleum ether
  4. custompurified by column chromatography (silica gel, methyl tert-butyl ether/ethyl acetate gradient)