HRID1436309

反应详情

EQUATION

反应方程式

HRID 1436309 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

3-Acetamido-4-nitrophthalic anhydride (1.3 g, 5.0 mmol) and 4-fluororesorcinol (1.3 g, 10 mmol) were added to methanesulfonic acid (10 ml), and the mixture was stirred at 80° C. under an argon atmosphere for 60 hours. The reaction mixture was added with water (120 ml) and refluxed for 2 hours. The reaction mixture was adjusted to pH 2, and precipitates were collected by filtration. The obtained product was dried and purified by silica gel chromatography (3% methanol/97% dichloromethane, v/v) to obtain the title compound (1.3 g, 61%).

WORKUP

后处理

  1. temperaturerefluxed for 2 hours
  2. customprecipitates
  3. filtrationwere collected by filtration
  4. customThe obtained product was dried
  5. custompurified by silica gel chromatography (3% methanol/97% dichloromethane, v/v)