反应详情

A solution of 4-fluoro-2-(5-methyl-1H-1,2,4-triazol-1-yl)benzonitrile (2.9 g, 14 mmol) in EtOH (100 mL) was mixed with 1N—HCl (15 mL) and 10% Pd—C (0.7 g, Aldrich). This mixture was hydrogenated in a Parr shaker at 45-55 psi of hydrogen for 20 h. The catalyst was filtered over Celite®, and washed with EtOH. The filtrate was concentrated, and the residue triturated with EtOH-Et2O to obtain 3.17 g (13 mmol, 91% yield) of the title compound as an off-white powder: HPLC 0.47 min (AP 100% at 254 nm); LC/MS m/z 207 (M+H); 1H NMR (DMSO-d6, 300 MHz) δ ppm 2.40 (3H, s, CH3), 3.77 (2H, d, J=5.5 Hz, NCH2), 7.52-7.62 (1H, m), 7.66 (1H, dd, J=9.2, 2.6 Hz), 7.87 (1H, t, J=7 Hz), 8.14 (1H, s), 8.47 (3H, brs, NH3+).

1. filtrationThe catalyst was filtered over Celite®
2. washwashed with EtOH
3. concentrationThe filtrate was concentrated
4. customthe residue triturated with EtOH-Et2O