反应详情

Sodium hydroxide (122 mg) was added into a cooled solution of 6-hydroxyflavanone (2 g) and hydroxylamine hydrochloride (900 mg) in ethanol (5 ml) and water (2 ml). Resulting mixture was refluxed for 6 hours and hydroxylamine hydrochloride (450 mg) and sodium hydroxide (61 mg) were added after every 45 min. After cooling into room temperature water (23 ml) and concentrated hydrochloric acid (5.6 ml) were added into the mixture. Precipitate was filtered, washed with water and dried in vacuum. 1H-NMR (400 MHz, d6-DMSO): 11.3 (s, 1H), 9.11 (s, 1H), 7.50-7.48 (m, 2H), 7.43-7.33 (m, 3H), 7.21 (d, 1H, J 2.9 Hz), 6.80 (d, 1H, J 8.8 Hz), 6.72 (dd, 1H, J 2.9, 8.8 Hz), 5.07 (dd, 1H, J 3.2, 11.9 Hz), 3.28 (dd, 1H, J 3.2, 17.1 Hz), 2.64 (dd, 1H, J 11.9,17.1 Hz).

1. customResulting mixture
2. temperaturewas refluxed for 6 hours
3. additionwere added into the mixture
4. filtrationPrecipitate was filtered
5. washwashed with water
6. customdried in vacuum