反应详情

温度

90 °C

To a 500 mL round bottom flask, 3-bromo-4-fluoraniline (5 g, 0.0261 mol), water (300 mL), chloral hydrate (5.19 g, 0.0314 mol), hydroxylamine hydrochloride (5.8 g, 0.0835 mol) and sodium sulphate (25 g) were added. To this reaction mixture, concentrated HCl (7.5 mL) was slowly added. The reaction mixture was stirred at 90° C. for 3 hours. A precipitate formed and was collected by filtration. The solid was dried to provide the title compound (4.2 g, 61%). 1H NMR (300 MHz, DMSO-d6): δ 12.28 (s, 1H), 10.51 (s, 1H), 8.12 (dd, J=2.4 Hz, J=2.7 Hz, 1H), 7.68 (m, 2H), 7.36 (t, J=8.7 Hz, 1H).

1. customA precipitate formed
2. filtrationwas collected by filtration
3. customThe solid was dried