反应详情

温度

30 °C

A mixture of 121a (86 mg, 0.15 mmol) and lithium hydroxide (36 mg, 1.5 mmol) in THF/i-propanol (5:3, 8 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 (5 mL). It was then extracted with ethyl acetate (2×10 mL). The combined ethyl acetate extract was concentrated under reduced pressure and the residue was purified by reverse-phase prep-HPLC to afford 121 (24 mg, 30%) as a white solid. MS-ESI: [M+H]+ 530.3. 1H NMR (500 MHz, CDCl3) δ 8.65 (d, J=5.0 Hz, 1H), 8.35 (d, J=2.0 Hz, 1H), 8.04 (d, J=2.5 Hz, 1H), 7.58-7.53 (m, 4H), 7.44 (s, 1H), 5.78 (s, 1H), 4.51-4.49 (m, 2H), 3.73 (s, 3H), 2.03 (s, 3H), 1.45 (s, 9H).

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