反应详情

To a solution of di-tert-butyl [5-(5-chloro-2-{4-[(2,4-dimethoxybenzyl)(1,2,4-thiadiazol-5-yl)sulfamoyl]-2,5-difluorophenoxy}phenyl)-1,2-benzoxazol-3-yl]imidodicarbonate (1.70 g, 1.92 mmol) in dichloromethane (25 mL) was added trifluoroacetic acid (10 mL). The reaction mixture was stirred at ambient temperature for 4 h and concentrated in vacuo. The residue was taken up in methanol (15 mL) and filtered. The filtrate was concentrated in vacuo and triturated with dichloromethane/diethyl ether (2:1 v/v, 15 mL) to afford 4-(2-(3-aminobenzo[d]isoxazol-5-yl)-4-chlorophenoxy)-2,5-difluoro-N-(1,2,4-thiadiazol-5-yl)benzenesulfonamide as a colorless solid in 63% yield (0.65 g): 1H NMR (300 MHz, DMSO-d6) δ8.49 (s, 1H), 7.95 (s, 1H), 7.72-7.66 (m, 1H), 7.62-7.59 (m, 2H), 7.49-7.42 (m, 2H), 7.26-7.24 (d, J=8.4 Hz, 1H), 7.14-7.08 (m, 1H), 6.47-6.40 (br s, 2H); MS (ES+) m/z 535.8 (M+1), 537.8 (M+1).

1. concentrationconcentrated in vacuo
2. filtrationfiltered
3. concentrationThe filtrate was concentrated in vacuo
4. customtriturated with dichloromethane/diethyl ether (2:1 v/v, 15 mL)