反应详情

A solution of b1 (12.38 g, 70.1 mmol) in 10% aqueous KOH (350 mL) was heated to reflux for 20 h and subsequently cooled to room temperature. The reaction mixture was acidified with 12 M HCl to pH 2-3, and the resulting precipitate was filtered, washed with water (2×50 mL), and dried under vacuum to afford c1 as a yellow solid (12.46 g, 92%): mp=151-155° C.; IR(cm−1) 2905 (br), 1736, 1652; 1H NMR (DMSO-d6) δ 2.34-2.29(m, 2H), 2.73 (t, 2H, J=7.6), 4.96-5.07 (m, 2H), 5.72-5.85 (m, 1H), 6.56 (d, 1H, J=7.5), 8.28 (d, 1H, J=7.5), 13.26 (s, br, 1H), 14.64 (s, br, 1H); Anal. C10H11NO3·0.10H2O: C, H, N.

1. temperatureto reflux for 20 h
2. filtrationthe resulting precipitate was filtered
3. washwashed with water (2×50 mL)
4. customdried under vacuum