反应详情

To a stirred solution of sodium sulfate (58.5 g, 412 mmol) in water (100 mL) was added a solution of chloralhydrate (9.36 g, 56.6 mmol) in water (120 mL). Chloroanisidine 215d (10 g, 51.5 mmol) was added followed by 37% HCl (20 mL). A solution of hydroxylamine (50% in water, 4.7 mL, 154.5 mmol) in 50 mL was then added and the reaction mixture was refluxed for 90 min. The suspended solid was filtered off, and washed with water and ether. Organics were dried over Na2SO4, filtered, and concentrated under reduced pressure to yield compound 245d as a brown solid. 1H NMR (DMSO-d6, 400 MHz) δ (ppm) 3.86 (s, 3H), 6.98 (d, J=8.07 Hz, 1H), 7.31 (t, J=8.07 Hz, 1H), 7.61 (d, J=8.07 Hz, 1H), 7.66 (s, 1H), 9.43 (s, 1H), 12.43 (s, 1H).

1. temperaturethe reaction mixture was refluxed for 90 min
2. filtrationThe suspended solid was filtered off
3. washwashed with water and ether
4. dry with materialOrganics were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure