反应详情

温度

35 °C

A mixture of 130b (100 mg, 0.18 mmol) and lithium hydroxide hydrate (189 mg, 4.5 mmol) in i-propanol/THF/water (2:2:1, 10 mL) was stirred at 35° C. for 30 min. The mixture was evaporated under reduced pressure and the residue was added water (5 mL). It was then extracted with dichloromethane (3×10 mL). The combined extract was concentrated under reduced pressure and the residue was purified by reverse-phase prep-HPLC to afford 130 (41.1 mg, 44.4%) as white solid. MS-ESI: [M+H]+ 530.3. 1H NMR (500 MHz, DMSO-d6) δ 8.56-8.53 (m, 2H), 7.90 (d, J=2.0 Hz, 1H), 7.78 (dd, J=2.0, 12.5 Hz, 1H), 7.61 (s, 1H), 7.51 (d, J=5.0 Hz, 1H), 7.41-7.39 (m, 2H), 7.37 (d, J=2.0 Hz, 1H), 6.97 (d, J=1.5 Hz, 1H), 5.04-5.02 (m, 1H), 4.41-4.39 (m, 2H), 3.59 (s, 3H), 3.58 (s, 3H), 1.39 (s, 9H).

1. customThe mixture was evaporated under reduced pressure
2. additionthe residue was added water (5 mL)
3. extractionIt was then extracted with dichloromethane (3×10 mL)
4. extractionThe combined extract
5. concentrationwas concentrated under reduced pressure
6. customthe residue was purified by reverse-phase prep-HPLC