反应详情

温度

100 °C

A mixture of 4-fluoro-3-(trifluoromethyl)benzonitrile (50.0 g, 0.26 mol, Combi-Blocks AN-1049) and 2-methylpiperidine (156 mL, 1.32 mol) in DMSO (500 mL) was heated at 100° C. under nitrogen for 12 hours. The reaction mixture was diluted with Et2O and washed with water, a saturated aqueous solution of NaHCO3 and a saturated aqueous solution of NH4Cl. The organic layer was dried (MgSO4) and the solvent was removed under reduced pressure to give the title compound as a beige powder. UPLC/MS, M−(ESI): 269.2. 1H NMR (DMSO-d6, 300 MHz) δ 8.19 (d, J=2.0 Hz, 1H), 8.12 (dd, J=8.4, 2.0 Hz, 1H), 7.75 (d, J=8.2 Hz, 1H), 3.13 (m, 1H), 2.88 (m, 1H), 2.56 (m, 1H), 1.77-1.25 (m, 6H), 0.72 (d, J=6.0 Hz, 3H).

1. washwashed with water
2. dry with materialThe organic layer was dried (MgSO4)
3. customthe solvent was removed under reduced pressure