反应详情

温度

30 °C

A mixture of 110a (100 mg, 0.15 mmol) and NaBH4 (20 mg, 0.45 mmol) in MeOH (30 mL) was stirred at 30° C. for 2 h. The mixture was quenched with water and extracted with EtOAc (10 mL×3). The combined EtOAc extract was concentrated under reduced pressure and the residue was purified by reverse-phase prep-HPLC to afford 110 (80 mg, 80%). MS: [M+H]+ 695.3. 1H NMR (500 MHz, CDCl3) δ 8.72 (d, J=2, 1H), 8.67 (d, J=5, 1H), 8.35 (d, J=2.5, 1H), 8.05 (d, J=3, 1H), 7.88 (s, 1H), 7.68 (d, J=2.5, 1H), 7.58-7.55 (m, 3H), 7.38-7.36 (m, 1H), 6.82 (d, J=8.5, 1H), 4.78-4.71 (m, 2H), 4.67-4.61 (m, 2H), 4.50 (s, 2H), 4.07 (t, J=6, 1H), 3.78-3.74 (m, 4H), 3.22-3.20 (m, 1H), 2.92 (d, J=3, 1H), 2.77-2.71 (m, 2H), 2.51-2.48 (m, 1H), 1.20-1.95 (m, 1H), 1.45 (s, 9H), 0.93-0.90 (m, 6H)

1. customThe mixture was quenched with water
2. extractionextracted with EtOAc (10 mL×3)
3. extractionThe combined EtOAc extract
4. concentrationwas concentrated under reduced pressure
5. customthe residue was purified by reverse-phase prep-HPLC