反应详情

温度

50 °C

A mixture of 108e (250 mg, 0.35 mmol) and LiOH (300 mg, 10 mmol) in iPrOH/THF (1:1, 3.5 mL) and H2O (1 mL) was stirred at 50° C. for 0.5 h. The mixture was evaporated in vacuo and the residue was extracted with Ethyl acetate (5 mL×2). The combined Ethyl acetate extract was concentrated under reduced pressure and the residue was purified with reverse-phase prep-HPLC to afford 108 (110 mg, 25%). LCMS: [M+H]+ 664. 1H NMR (500 MHz, DMSO) δ 9.33 (s, 1H), 8.67 (s, 1H), 8.55-8.54 (m, 2H), 7.95 (d, J=3.0, 1H), 7.44-7.41 (m, 2H), 7.37-7.33 (m, 2H), 6.53 (s, 1H), 4.98 (t, J=5.0, 1H), 4.55-4.54 (m, 2H), 4.45-4.44 (m, 2H), 4.13-4.32 (m, 5H), 3.91 (s, 1H), 3.43-3.41 (m, 1H), 3.10 (s, 4H), 2.60-2.38 (m, 8H), 1.78-1.76 (m, 2H), 1.69-1.67 (m, 2H)

1. customThe mixture was evaporated in vacuo
2. extractionthe residue was extracted with Ethyl acetate (5 mL×2)
3. extractionThe combined Ethyl acetate extract
4. concentrationwas concentrated under reduced pressure
5. customthe residue was purified with reverse-phase prep-HPLC