Reaction Steps
Dissolve 4-fluoro-N-methyl-N-(1-(4-(1-methyl-1H-pyrazol-5-yl)phthalazin-1-yl)piperidin-4-yl)-2-(trifluoromethyl)benzamide (7.13 g, 13.91 mmol) in dichloromethane (100 mL) and add excess 1 N HCl in diethyl ether (30 mL, 30 mmol). Remove the solvents under reduced pressure to provide the title compound (7.05 g, 92%). ES/MS m/z 513.0 (M+1). NMR showed a 2:1 mixture of amide rotamers. Major rotamer; 1H NMR (400 MHz, DMSO-d6): δ 8.34 (m, 1H), 8.26 (m, 2H), 7.95 (m, 1H), 7.75 (m, 1H), 7.64 (m, 2H), 7.55 (m, 1H), 6.72 (d, 1H, J=2Hz), 5.15 (br, 1H), 4.71 (m, 1H), 4.22 (m, 2H), 3.84 (s, 3H), 3.48 (m, 2H), 2.65 (s, 3H), 2.19 (m, 2H), 1.89 (m, 2H). Minor rotamer; 1H NMR (400 MHz, DMSO-d6): δ 8.27 (m, 1H), 8.24 (m, 2H), 7.94 (m, 1H), 7.73 (m, 1H), 7.63 (m, 3H), 6.70 (d, 1H, J=2 Hz), 5.15 (br, 1H), 4.71 (m, 1H), 4.07 (m, 2H), 3.81 (s, 3H), 3.16 (m, 2H), 2.92 (s, 3H), 1.90 (m, 2H), 1.62 (m 2H).
