反应详情

温度

90 °C

To a solution of Intermediate 1B (11.9 g, 35 mmol) in anisole (24 mL) was added TFA (24 mL). The reaction mixture was stirred at 90° C. for 6 h and the solvent was removed under reduced pressure. The residue was suspended in MeOH (50 mL) and then treated with NaHCO3 (3.3 g, 39 mmol) in water (200 mL). The mixture was stirred at rt for 15 min and the pH was checked to be 9-10. The precipitate was collected by filtration and washed with water to afford Intermediate 1C (6.0 g, 91%). 1H NMR (400 MHz, DMSO-d6) δ 7.20 (d, J=5.7 Hz, 1H), 7.36 (s, 2H), 7.95 (d, J=5.7 Hz, 1H), 8.15 (dd, J=9.2, 2.6 Hz, 1H), 8.43 (d, J=9.2 Hz, 1H), 8.67 (d, J=2.6 Hz, 1H).

1. customthe solvent was removed under reduced pressure
2. stirringThe mixture was stirred at rt for 15 min
3. filtrationThe precipitate was collected by filtration
4. washwashed with water