反应详情

9-Chloro-2,3-dihydro-[1,4]dioxino[2,3-f]quinolin-10-ol (3.12 g, 13.1 mmol) in dry DMF (16.7 mL) was cooled in ice and phosphorus tribromide (4.78 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 2 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 (3.55 g, 90%). LC/MS (ES) m/z 300 (MH+ 100%); 1H-NMR (400 MHz, DMSO), 8.73 (1H, s, CHNHC), 7.62 (1H, d, J=9.12, CHCOCH2), 7.47 (1H, d, J=9.08, CHCN), 4.43 (4H, m, 2×(CH2O)).

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