反应详情

温度

35 °C

2,3-Dihydro-7H-[1,4]dioxino[2,3-f]quinolin-10-one (6.93 g, 34.1 mmol, 1 eq) in acetic acid (95.9 mL) was sonicated and warmed until all had dissolved, and then it was treated with N-chlorosuccinimide (5.01 g, 37.5 mmol, 1.1 eq) and the mixture was heated at 35° C. for 18 hr, cooled and the solid collected and washed with acetic acid and dried in vacuo at 40 oC overnight, to give a white solid (5.93 g, 73%). LC/MS (ES) m/z 237 (MH+ 84%); 1H-NMR (400 MHz, d6-DMSO), 8.17 (1H, d, J=6.28, CHNHC), 7.21 (1H, d, J=8.96 Hz, CHCO), 7.01 (1H, d, J=9, CHCN), 4.29-4.25 (4H, m, 2×(CH2O)).

1. temperaturewarmed until
2. dissolutionall had dissolved
3. temperaturecooled
4. customthe solid collected
5. washwashed with acetic acid
6. customdried in vacuo at 40 oC overnight