HRID1167191

反应详情

EQUATION

反应方程式

HRID 1167191 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

64 g (397 mmol) of 8-hydroxyquinoline N-oxide, 550 ml of acetic anhydride and 40 ml of acetic acid are placed in a 1 l round-bottomed flask. The reaction mixture is heated at reflux (135° C.) for 24 h, 40 ml of acetic acid are then again added and heating is continued for 1 h 30. The reaction mixture is allowed to return to ambient temperature and 400 ml of toluene are added. A precipitate appears and is filtered off. A further 400 ml of toluene are added and filtration is carried out. The precipitate is washed with 200 ml of ethyl ether and is dried in a desiccator under vacuum over phosphorus pentoxide to provide to provide 70.5 g of 2-acetoxy-8-hydroxyquinoline in the form of a brown solid. (Yield: 88%)

WORKUP

后处理

  1. temperatureThe reaction mixture is heated
  2. temperatureheating
  3. customto return to ambient temperature
  4. filtrationis filtered off
  5. additionA further 400 ml of toluene are added
  6. filtrationfiltration
  7. washThe precipitate is washed with 200 ml of ethyl ether
  8. dry with materialis dried in a desiccator under vacuum over phosphorus pentoxide
  9. customto provide