反应详情

温度

160 °C

4-Chloro-6,7-dimethoxyquinoline (58.2 mg), 5-fluoro-2-hydroxyacetophenone (409 mg), and 4-dimethylaminopyridine (317 mg) were suspended in o-dichlorobenzene (5 ml), and the suspension was stirred at 160° C. for 8 hr. The reaction solution was cooled to room temperature, and the solvent was then removed therefrom by distillation under the reduced pressure. Chloroform was added to the residue, and the organic layer was washed with a 1 N aqueous potassium hydroxide solution and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed therefrom by distillation under the reduced pressure, and the residue was purified by column chromatography using chloroform and by thin layer chromatography using acetone-hexane to give the title compound (63.5 mg, yield 72%).

1. temperatureThe reaction solution was cooled to room temperature
2. customthe solvent was then removed
3. distillationby distillation under the reduced pressure
4. additionChloroform was added to the residue
5. washthe organic layer was washed with a 1 N aqueous potassium hydroxide solution and saturated brine
6. dry with materialwas dried over anhydrous sodium sulfate
7. customThe solvent was removed
8. distillationby distillation under the reduced pressure
9. customthe residue was purified by column chromatography