反应详情

温度

120 °C

To phosphorous oxychloride (2.02 mL, 21.6 mmol) was added quinoline (1.34 mL, 11.2 mmol) followed by 3-bromo-5-trifluoromethyl-2(1H)-pyridone (5.0 g, 20.07 mmol). The mixture was heated at 120° C. for 3 hrs, then cooled to 100° C., whn water (10 mL) was carefully added. After cooling to room temperature, saturated sodium bicarbonate was added (100 mL) and the mixture extracted with ethyl acetate (2×100 mL). The extracts were dried (MgSO4) and concentrated, and the residue purified by silica chromatography to give the product as a liquid (4.05 g, 15.5 mmol, 75% yield).

1. temperaturecooled to 100° C.
2. temperatureAfter cooling to room temperature
3. extractionthe mixture extracted with ethyl acetate (2×100 mL)
4. dry with materialThe extracts were dried (MgSO4)
5. concentrationconcentrated
6. customthe residue purified by silica chromatography