HRID228844

反应详情

EQUATION

反应方程式

HRID 228844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

2,3-Dihydroxyquinoline (450 mg), 4-chloro-6,7-dimethoxyquinoline (575 mg), and 4-dimethylaminopyridine (472 mg) were suspended in o-dichlorobenzene (12 ml), and the mixture was stirred at 135° C. for 5.5 hr. The reaction solution was cooled to room temperature, water was then added to the reaction solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and saturated brine and was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography using acetone-chloroform to give 3-(6,7-dimethoxy-quinolin-4-yloxy)-quinolin-2-ol (344 mg, yield 77%).

WORKUP

后处理

  1. temperatureThe reaction solution was cooled to room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe ethyl acetate layer was then washed with water and saturated brine
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. customThe solvent was removed by distillation under the reduced pressure
  6. customThe residue was purified by column chromatography