反应详情

3-Acetylbenzoic acid (10.0 g, 60.9 mmol), hydroxylamine hydrochloride (33.9 g, 487.4 mmol) and sodium acetate (45.0 g, 548.3 mmol) were suspended in ethanol (115 mL) and water (115 mL) and the mixture heated at reflux for 30 minutes. The solvents were removed under reduced pressure, and the residue was triturated with water. The resulting precipitate was isolated by filtration and dried in vacuo to give the sub-title compound as a white solid (10.34 g, 95% yield). 1H NMR (400 MHz, DMSO) δ 2.18 (s, 3H), 7.52 (t, 1H), 7.88 (dd, 1H), 7.91-7.95 (m, 1H), 8.22 (s, 1H), 11.36 (s, 1H) and 12.86 (s, 1H); MS (ES+) 180.3.

1. temperatureat reflux for 30 minutes
2. customThe solvents were removed under reduced pressure
3. customthe residue was triturated with water
4. customThe resulting precipitate was isolated by filtration
5. customdried in vacuo