反应详情

温度

70 °C

1 N aqueous NaOH solution (1.56 mL) was added to the solution of 37 (57 mg, 0.15 mmol) in MeOH (25 mL). The mixture was stirred at 70° C. for 1 h. The solvent was evaporated to give a crude product, which was purified by silica gel column chromatography using CH2Cl2/MeOH (3:1, v/v) to afford 44 (55 mg, 87%) as a white powder. mp 220° C. (decomp.); 1H NMR (DMSO-d6) δ 8.39 (s, 1H, H4), 7.54 (s, 1H, H6), 6.89 (d, 1H, H5′, J=8.7 Hz), 6.73 (d, 1H, H2′, J=1.5 Hz), 6.63 (dd, 1H, H6′, J=1.5, 8.7 Hz), 6.05 (AB, 2H, 3′,4′-OCH2O—, Δδ=18.9 Hz), 5.81 (AB, 2H, 7,8-OCH2O—, A5=8.1 Hz), 4.12 (s, 2H, 2-CH2OH); MS (FAB, positive) m/z 425 [M+H+2]+, 423 [M+H]+.

1. customThe solvent was evaporated
2. customto give a crude product, which
3. customwas purified by silica gel column chromatography