反应详情

To a solution of (3S,4S)-4-(aminomethyl)-1-{2-[3-fluoro-6-(methyloxy)-1,5-naphthyridin-4-yl]ethyl}-3-pyrrolidinol (225 mg, 0.703 mmol) in DIPEA (188 μL, 1.05 mmol) and DCM (7 mL) at 0° C. was added 3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-sulfonyl chloride (210 mg, 0.845 mmol) in one portion. The solution stirred for 0.5 h and was concentrated. The resulting residue was purified by column chromatography (silica, 2-4% MeOH in DCM (1% NH OH)) yielding the title compound (290 mg, 75%) as a white foam: LC/MS (ES) m/e 548 (M+H); H NMR (CD OD, 400 Hz) δ 8.65 (s, 1H), 8.22 (d, J=9.1 Hz, 1H), 7.53 (d, J=8.0 Hz, 1H), 7.45-7.48 (m, 2H), 7.20 (d, J=9.1 Hz, 1H), 4.28-4.31 (m, 1H), 4.14 (s, 3H), 3.55 (s, 2H), 3.42-3.46 (m, 2H), 3.21-3.23 (m, 1H), 3.05-3.15 (m, 1H), 2.91-3.05 (m, 2H), 2.86-2.90 (m, 2H), 2.51-2.62 (m, 2H), 2.33-2.4 (m, 1H).

1. concentrationwas concentrated
2. customThe resulting residue was purified by column chromatography (silica, 2-4% MeOH in DCM (1% NH OH))