反应详情

3-Chloro-6-methoxy-quinolin-4-ol from above in dry DMF (80 mL) was cooled in ice and phosphorus tribromide (15.6 mL) added drop-wise, and the mixture was stirred, with ice-cooling for 30 minutes then allowed to warm to room temperature and stirred for a further 3.5 hours. It was cooled in ice and sodium carbonate solution was added and the solid was collected, washed well with water, and dried in vacuo, to afford a pale yellow solid (13.2 g). MS (ES) m/z 272/274/276 (M+H)+.

1. temperaturecooling for 30 minutes
2. stirringstirred for a further 3.5 hours
3. temperatureIt was cooled in ice
4. customthe solid was collected
5. washwashed well with water
6. customdried in vacuo