反应详情

温度

85 °C

1-(6-Bromo-4-hydroxyquinolin-3-yl)-2-methylpropan-1-one (16.0 g, 54.4 mmol) was added to phosphoryl chloride (160 mL) and the reaction was stirred at 85° C. for 1.5 h. The reaction mixture was cooled and slowly poured into a 2:1 solution of satd. aq. sodium bicarbonate/ethyl acetate at 0° C. The organic layer was separated and was washed with satd. aq. sodium bicarbonate and brine, dried over anhydrous sodium sulfate, filtered, and concentrated to afford the desired product (14.8 g, 89%) as a yellow solid: ESI MS m/z 312 [C13H11BrClNO+H]+.

1. temperatureThe reaction mixture was cooled
2. additionslowly poured into a 2:1 solution of satd
3. customat 0° C
4. customThe organic layer was separated
5. washwas washed with satd
6. dry with materialaq. sodium bicarbonate and brine, dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated