反应详情

温度

70 °C

To a suspension of 3-[4-[(2,4-difluorobenzyl)oxy]-2-methyl-6-oxopyrimidin-1(6H)-yl]-4-methylbenzoic acid (1.0 g, 2.6 mmol) in anhydrous acetonitrile (15 mL) was added N-chlorosuccinimide (0.38 g, 2.9 mmol) and dichloroacetic acid (0.2 mL, 2.6 mmol). The reaction was heated in oil bath (70° C.) overnight under nitrogen. The reaction mixture was concentrated under reduced pressure to remove acetonitrile. The resulting residue was washed with water for 30 min, filtered, and rinsed with water. The white solid (830 mg, 82%) was dried in vacuo. 1H-NMR (CD3OD, 400 MHz) δ 8.09 (dd, 1H, J=1.6 Hz), 7.88 (d, 1H, J=2 Hz), 7.56 (m, 2H), 7.01 (m, 2H), 5.57 (s, 2H), 2.16 (s, 3H), 2.13(s, 3H); ES-HRMS m/z 421.0753 (M+H C20H16ClF2N2O4 requires 421.0761).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. customto remove acetonitrile
3. washThe resulting residue was washed with water for 30 min
4. filtrationfiltered
5. washrinsed with water
6. dry with materialThe white solid (830 mg, 82%) was dried in vacuo