反应详情

A solution of 25.0 g (150 mmol) of 4-(hydroxymethyl)benzonitrile, 20.8 g (300 mmol) of hydroxyamine hydrochloride and 50.4 g (600 mmol) of sodium bicarbonate in 250 mL of methanol was heated to reflux and stirred for 20 h. The reaction mixture was cooled to rt and filtered. The solid was washed with 100 mL of methanol. The combined methanol solution was concentrated to dryness to afford 31.0 g (99%) of the title compound: 1H NMR (400 Mhz, CD3OD) δ 4.63 (s, 2H), 7.39 (d, J=8.0, 2H), 7.62 (d, J=8.0, 2H).

1. temperatureto reflux
2. filtrationfiltered
3. washThe solid was washed with 100 mL of methanol
4. concentrationThe combined methanol solution was concentrated to dryness