反应详情

To a solution of di-tert-butyl (5-hydroxy-1,2-benzoxazol-3-yl)imidodicarbonate (0.40 g, 1.1 mmol) in dimethyl sulfoxide (5 mL) was added N-(2,4-dimethoxybenzyl)-2,4,5-trifluoro-N-(1,2,4-thiadiazol-5-yl)benzenesulfonamide (0.50 g, 1.1 mmol) and potassium carbonate (0.19 g, 1.4 mmol). The reaction was stirred at ambient temperature for 18 h, diluted with ethyl acetate (10 mL), washed with water (3×10 mL), dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford di-tert-butyl (5-{4-[(2,4-dimethoxybenzyl)(1,2,4-thiadiazol-5-yl)sulfamoyl]-2,5-difluorophenoxy}-1,2-benzoxazol-3-yl)imidodicarbonate as a colorless solid in 87% yield (1.09 g): 1H NMR (300 MHz, CDCl3) δ8.17 (s, 1H), 7.66-7.59 (m, 2H), 7.30-7.26 (m, 2H), 7.18-7.16 (m, 1H), 6.45-6.40 (m, 1H), 6.35 (d, J=8.1 Hz, 1H), 6.37 (s, 1H), 2.60 (s, 2H), 3.75 (s, 3H), 3.70 (s, 3H), 1.56 (s, 9H), 1.40 (s, 9H); MS (ES+) m/z 775.8 (M+1).

1. washwashed with water (3×10 mL)
2. dry with materialdried over anhydrous sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo