反应详情

温度

50 °C

Hydrogen peroxide (30 wt. % solution in water, 45 mL) was added to a solution of a1 (12.13 g, 70.2 mmol) in a mixture of EtOH (150 mL) and 10% aqueous NaOH (280 mL) at 23° C. The reaction mixture was heated to 50° C. for 18 h, then was cooled to 23° C. and the volatiles were removed under reduced pressure. The residue was acidified with 12 M HCl to pH 2-3, and the resulting precipitate was filtered, washed with water (2×50 mL), and air-dried to afford b1 as a yellow solid (13.48 g, 100%): mp=195-198° C.; IR (cm−1) 3329, 3134, 1688, 1642; 1H NMR (DMSO-d6) δ 2.31-2.38 (m, 2H), 2.64 (t, 2H, J=7.6), 4.96-5.05 (m, 2H), 5.71-5.84 (m, 1H), 6.29 (d, 1H, J=7.3), 7.45 (s, br, 1H), 8.21 (d, 1H, J=7.3), 9.00 (s, br, 1H), 12.37 (s, br, 1H); Anal. C10H12N2O2·0.15H2O: C, H, N.

1. temperaturewas cooled to 23° C.
2. customthe volatiles were removed under reduced pressure
3. filtrationthe resulting precipitate was filtered
4. washwashed with water (2×50 mL)
5. customair-dried