反应详情

温度

25 °C

A mixture of 112a (140 mg, 0.20 mmol), NaBH4 (21 mg, 0.60) and CH3OH (8 mL) was stirred at 25° C. for 1 h. Then the reaction mixture was quenched with water (10 mL), the mixture was extracted with CH2Cl2 (15 mL×2). The combined CH2Cl2 extract was concentrated under reduced pressure. The residue was purified with reverse-phase prep-HPLC to afford 112 (70 mg, 50%). LCMS: [M+H]+ 695. 1H NMR (500 MHz, DMSO) δ 8.50-8.60 (m, 2H), 8.44 (s, 1H), 7.90 (d, J=1.5, 1H), 7.82 (d, J=3.0, 1H), 7.75-7.78 (m, 1H), 7.51-7.53 (m, 1H), 7.45 (d, J=2.5, 1H), 7.33-7.35 (m, 1H), 7.22-7.24 (m, 1H), 4.47-4.59 (m, 2H), 4.36-4.45 (m, 4H), 3.60 (s, 3H), 3.46-3.50 (m, 1H), 3.38-3.41 (m, 3H), 3.14-3.17 (m, 1H), 2.96-3.00 (m, 1H), 2.60-2.64 (m, 1H), 2.50-2.55 (m, 1H), 2.14-2.17 (m, 1H), 2.06-2.10 (m, 1H), 1.66-1.69 (m, 1H), 1.39 (s, 9H), 1.21-1.28 (m, 1H), 0.77-0.80 (m, 3H)

1. customThen the reaction mixture was quenched with water (10 mL)
2. extractionthe mixture was extracted with CH2Cl2 (15 mL×2)
3. extractionThe combined CH2Cl2 extract
4. concentrationwas concentrated under reduced pressure
5. customThe residue was purified with reverse-phase prep-HPLC