反应详情

1-(5-Fluoro-2-methoxy-4-(4-methyl-2-oxopyridin-1(2H)-yl)phenyl)-N-(isoxazol-3-yl)-N-(4-methoxybenzyl)-2-oxo-1,2-dihydroquinoline-6-sulfonamide (18 mg, 0.028 mmol) was taken up in TFA (2 mL) in a microwave vial and irradiated to 70° C. for 1 h. Concentration under a stream of N2 followed by column chromatography (5 g Redisep gold column, 0-80% [3:1 EtOAc/EtOH]/hept gradient with 10% DCM) afforded 1-(5-fluoro-2-methoxy-4-(4-methyl-2-oxo-1(2H)-pyridinyl)phenyl)-N-3-isoxazolyl-2-oxo-1,2-dihydro-6-quinolinesulfonamide (0.24 mg, 0.459 μmol, 1.640% yield) as a colorless residue. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 2.55 (s, 3 H) 3.72 (s, 3 H) 6.64 (d, J=1.76 Hz, 1 H) 6.88 (d, J=9.74 Hz, 1 H) 6.98-7.02 (m, 2 H) 7.11 (d, J=6.84 Hz, 1 H) 7.32 (d, J=1.35 Hz, 2H) 7.80-7.90 (m, 2 H) 8.15 (d, J=2.07 Hz, 1 H) 8.23 (d, J=5.39 Hz, 1 H) 8.29 (d, J=1.66 Hz, 1 H). m/z (ESI) 523.0 (M+H)+.

1. customirradiated to 70° C. for 1 h
2. concentrationConcentration under a stream of N2