HRID220818

反应详情

EQUATION

反应方程式

HRID 220818 的结构方程式

PROCEDURE

实验过程

A solution of 2-chloro-4-hydroxy-benzonitrile (5.0 g, 32.6 mmol) in ethanol (125 ml) was treated with conc. sulphuric acid (25 ml) and the mixture heated at reflux for 3 days. Conc. sulphuric acid (25 ml) was added and the mixture was heated at reflux for another 2 days. The volatiles were removed in vacuo, and the aqueous residue was basified with saturated NaHCO3 and extracted 4 times with diethyl ether. The combined organic extracts were dried and concentrated in vacuo to yield the title compound (2.5 g, 38%).

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 3 days
  3. temperaturethe mixture was heated
  4. temperatureat reflux for another 2 days
  5. customThe volatiles were removed in vacuo
  6. extractionextracted 4 times with diethyl ether
  7. customThe combined organic extracts were dried
  8. concentrationconcentrated in vacuo