反应详情

Compound 11 (0.473 g, 2.25 mmol, 1.00 eq) was dissolved in ethanol (10 mL) and 1N NaOH (5 mL) was added. The mixture was refluxed for 18 h and after cooling the reaction was neutralized with 1N HCl (5 mL) and the reaction was concentrated in vacuo. The crude reaction was dissolved in 10% MeOH/CH2Cl2 and the undissolved salt was filtered off and the solvents were removed in vacuo to afford 0.461 g (89%) of the title compound as a tan solid: 1H NMR (400 MHz, CDCl3) δ8.65-8.61 (m, 2H), 8.12 (d, J=6.7 Hz, 1H), 7.88 (ddd, J=8.1, 2.5, 1.6 Hz, 1H), 7.60 (dd, J=8.2, 4.8 Hz 1H), 7.4 (d, J=2.9 Hz, 1H), 6.88 (dd, J=6.7, 2.9 Hz, 1H), 3.46 (s, 3H); [M+1]+: 230.2.

1. temperatureThe mixture was refluxed for 18 h
2. temperatureafter cooling the reaction
3. concentrationthe reaction was concentrated in vacuo
4. customThe crude reaction
5. filtrationthe undissolved salt was filtered off
6. customthe solvents were removed in vacuo