反应详情

To a flask charged with 2-Fluoro-5-[2-(2-oxopiperazin-1-yl)ethyl]benzonitrile (53 mg, 0.25 mmol) and Fluoro(1-oxo-1,3-dihydro-2-benzofuran-5-yl)acetaldehyde (20 mg, 0.10 mmol) was added NaBH(OAc)3 (153 mg, 0.72 mmol). The mixture was stirred at RT for 12 hours. Then the reaction was diluted with DCM (120 mL), washed with brine (15 mL), dried over Na2SO4 and concentrated. The residue was purified with prep-TLC (MeOH/DCM=1:15) to obtain the title product. 1H-NMR (400 MHz, MeOD) δ ppm 7.88 (d, J=8.0 Hz, 1H), 7.55-7.65 (m, 4H), 7.25 (t, J=9.0 Hz, 1H), 5.90 (dd, J=7.6, 3.2 Hz, 1H), 5.78 (dd, J=7.6, 3.2 Hz, 1H), 5.39 (s, 2H), 3.59 (d, J=7.6, 7.0 Hz, 2H), 2.80-2.95 (m, 6H).

1. washwashed with brine (15 mL)
2. dry with materialdried over Na2SO4
3. concentrationconcentrated
4. customThe residue was purified with prep-TLC (MeOH/DCM=1:15)