反应详情

(2R,4S)-Methyl 2-(3-fluoro-4-(trifluoromethyl)benzyl)-4-(3-oxo-2,3-dihydroisoxazol-5-yl)piperidine-1-carboxylate (594 mg, 1.48 mmol) was dissolved in hydrogen bromide (33% in acetic acid, 10 mL, 57.10 mmol) and the mixture stirred at room temperature overnight. The solvent was evaporated and the residue purified by preparative HPLC (Instrument: FractionLynx III, Mobilphase: gradient 5-95% MeCN in 0.2% NH3, pH10, Column: Xbridge Prep C18 5 μm OBD 19*150 mm) to yield 5-((2R,4S)-2-(3-fluoro-4-(trifluoromethyl)benzyl)-piperidin-4-yl)isoxazol-3(2H)-one (338 mg, 66%). 1H NMR (600 MHz, dmso) δ 1.08 (q, 1H), 1.32 (qd, 1H), 1.71-1.79 (m, 2H), 2.45-2.72 (m, 4H), 2.72-2.80 (m, 1H), 2.96 (d, 1H), 5.68 (s, 1H), 7.23 (d, 1H), 7.35 (d, 1H), 7.65 (t, 1H). HRMS Calculated for [C16H16F4N2O2+H]+: 345.1226. Found: 345.1232

1. customThe solvent was evaporated
2. customthe residue purified by preparative HPLC (Instrument: FractionLynx III, Mobilphase: gradient 5-95% MeCN in 0.2% NH3, pH10, Column: Xbridge Prep C18 5 μm OBD 19*150 mm)