反应详情

温度

120 °C

8-Bromo-7-(trifluoromethyl)imidazo[1,2-a]quinoxalin-4(5H)-one (9.4 g, 0.0283 mol) is stirred under nitrogen with N,N-dimethylaniline (14.5 mL, 0.1123 mol) and phosphoryl chloride (190 mL, 2.0119 mol) at reflux (120° C.) for 1.5 hour. After cooling down to room temperature, the mixture is slowly poured in a mixture of water (2 L) and sodium hydroxide 5N (1 L) below 10° C. The mixture is extracted four times with ethyl acetate (200 mL) and the combined organic phases are washed with water (200 mL), dried over sodium sulfate and concentrated to about 100 mL. Cyclohexane (500 mL) is added at room temperature. The mixture is cooled to 0-5° C. and filtered. The cake is washed with cyclohexane and dried under vacuum to afford the title compound as a yellow solid (7.98 g, 80.4%)

1. temperatureAfter cooling down to room temperature
2. extractionThe mixture is extracted four times with ethyl acetate (200 mL)
3. washthe combined organic phases are washed with water (200 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated to about 100 mL
6. additionCyclohexane (500 mL) is added at room temperature
7. temperatureThe mixture is cooled to 0-5° C.
8. filtrationfiltered
9. washThe cake is washed with cyclohexane
10. customdried under vacuum