反应详情

The compound 1 (0.1 g, 0.32 mmol) is dissolved in ethanol (0.5 mL), and 10% of sodium hydroxide aqueous solution (0.5 mL) is added into. The resulting mixture is reacted for 1 hour with reflux. After cooling, the strong hydrochloric acid (0.3 mL) is added and followed by stirring for 10 minutes. 5 mL of water is added, and produced solid is obtained by filtration. The filter cake is washed with water, followed by drying to obtain 0.09 g of the captioned compound, yield: 90%. m.p. 196-197° C. 1H NMR (DMSO-d6): δ=5.25(s, 2 H), 7.08(dd, J=2.2 Hz, 8.8 Hz, 1H), 7.12(d, J=2.2 Hz, 1H), 7.30-7.50(m, 5H), 7.83(d, J=8.8 Hz, 1H), 8.73(s, 1H); Elements Analysis, C17H12O5 (296): Calculated C, 68.92; H, 4.05; Found C, 68.50; H, 4.12; IR(KBr) : 3054.7, 1747.2, 1677.8, 1600.7, 1556.3, 1421.3, 1378.9, 1257.4, 1209.2, 1120.2, 732.8 cm−1; EI-MS(m/z): 296(4, M+), 91(100).

1. customThe resulting mixture is reacted for 1 hour
2. temperaturewith reflux
3. temperatureAfter cooling
4. customproduced solid
5. customis obtained by filtration
6. washThe filter cake is washed with water
7. customby drying