反应详情

To a solution of compound 3b (0.37 g, 1 mmol) in THF (10 mL) was added LiOH (35 mg, 1.5 mmol) followed by 2 mL of water at room temperature. The reaction mixture was stirred overnight. The reaction was quenched by adding 1N HCl. The solvent was evaporated in vacuo. The resulting white solids were collected by suction filtration and washed with water. The crude product was recrystallized from MeOH to give the titled compound (0.33 g, 96% yield) as a white solid. mp 188.5-190.9° C. 1H NMR (300 MHz, DMSO-d6): δ 13.10 (s, 1H), 7.87 (d, J=8 Hz, 2H), 7.55-7.48 (m, 4H), 7.44-7.37 (m, 3H), 7.34-7.26 (m, 2H), 7.10 (s, 1H).

1. customThe reaction was quenched
2. additionby adding 1N HCl
3. customThe solvent was evaporated in vacuo
4. filtrationThe resulting white solids were collected by suction filtration
5. washwashed with water
6. customThe crude product was recrystallized from MeOH