HRID228706

反应详情

EQUATION

反应方程式

HRID 228706 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

4-Chloro-2-hydroxyacetophenone (45 mg), 4-chloro-6,7-dimethoxyquinoline (60 mg), and 4-dimethylaminopyridine (95 mg) are suspended in o-dichlorobenzene (10 ml) to prepare a suspension which was then stirred at 120° C. overnight and then at 140° C. for 5 hr. The reaction solution was cooled to room temperature, and the solvent was removed by distillation under the reduced pressure. Water was then added to the residue, and the mixture was extracted with chloroform. The chloroform layer was washed with water and was dried over anhydrous sodium sulfate, and the solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using acetone-hexane to give the title compound (11 mg, yield 12%).

WORKUP

后处理

  1. customto prepare a suspension which
  2. waitat 140° C. for 5 hr
  3. temperatureThe reaction solution was cooled to room temperature
  4. customthe solvent was removed by distillation under the reduced pressure
  5. additionWater was then added to the residue
  6. extractionthe mixture was extracted with chloroform
  7. washThe chloroform layer was washed with water
  8. dry with materialwas dried over anhydrous sodium sulfate
  9. customthe solvent was removed by distillation under the reduced pressure
  10. customthe residue was purified by thin layer chromatography