HRID1831038

反应详情

EQUATION

反应方程式

HRID 1831038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
165 °C

PROCEDURE

实验过程

A mixture of 4-aminophenol (3.27 g, 30.0 mmol) and 3,3-dimethylglutaric anhydride (4.26 g, 30.0 mmol) was heated in a round bottom flask at 165° C. for 1 h, followed by heating at 180° C. for 7 h. After cooling to room temperature the solid material was dissolved in hot ethanol, activated charcoal was added and the solution was heated at reflux for 1 h. The solid material was removed by hot filtration. The solvent was evaporated and the residue was crystallised (water/ethanol) yielding the title compound (3.51 g, 50%, pink solid).

WORKUP

后处理

  1. temperatureby heating at 180° C. for 7 h
  2. temperatureAfter cooling to room temperature the solid material
  3. temperaturethe solution was heated
  4. temperatureat reflux for 1 h
  5. customThe solid material was removed by hot filtration
  6. customThe solvent was evaporated
  7. customthe residue was crystallised (water/ethanol)