反应详情

温度

30 °C

A mixture of 160b (120 mg, 0.21 mmol) and lithium hydroxide monohydrate (88 mg, 2.1 mmol) in THF/i-propanol (4:2, 6 mL) and water (2 mL) was stirred at 30° C. for 1 h. The mixture was evaporated under reduced pressure and the residue was diluted with water (10 mL). It was then extracted with ethyl acetate (2×20 mL). The combined ethyl acetate extract was concentrated under reduced pressure and the residue was purified by reverse-phase prep-HPLC to afford 160 (50 mg, 45%) as a white solid. MS-ESI: [M+H]+ 527.8. 1H NMR (500 MHz, CHCl3) δ 8.78 (d, J=2.5 Hz, 1H), 8.71 (d, J=5.0 Hz, 1H), 8.36 (d, J=2.0 Hz, 1H), 8.31 (s, 1H), 8.19 (s, 1H), 8.14 (s, 1H), 8.05 (d, J=2.0 Hz, 1H), 7.81 (d, J=2.5 Hz, 1H), 7.59 (s, 1H), 7.56-7.55 (m, 2H)

1. customThe mixture was evaporated under reduced pressure
2. additionthe residue was diluted with water (10 mL)
3. extractionIt was then extracted with ethyl acetate (2×20 mL)
4. extractionThe combined ethyl acetate extract
5. concentrationwas concentrated under reduced pressure
6. customthe residue was purified by reverse-phase prep-HPLC