反应详情

温度

60 °C

N-benzenesulfonyl-4-acetylamino-3-(2,4-difluorobenzylamino)benzamide (0.370 g) is added to a mixture solvent of 10% hydrochloric acid (3.3 g), methanol (6 ml), and water (4 ml). Furthermore, 35% hydrochloric acid (0.5 g) is added and the solution is stirred for three hours at 60° C. After 20% potassium bicarbonate aqueous solution is added to turn the reaction solution into a basic, its acidity is adjusted to pH 5˜6 with 10% hydrochloric acid. Precipitated crystals are separated through filtration, dried and thus, 0.182 g of 6-benzenesulfonylcarbamoyl-1-(2,4-difluorobenzyl)-2-methyl-benzimidazole is obtained. 1H-NMR (DMSO-d6, δ): 2.53 (3H, s), 5.56 (2H, s), 6.95-7.01 (1H, m), 7.04 (1H, dt, J=8.7 and 1.4 Hz), 7.32 (1H, dt, J=10.7 and 2.1 Hz), 7.59-7.66 (3H, m), 7.68-7.74 (2H, m), 8.00 (2H, d, J=8.1 Hz), 8.13 (1H, s), 12.43 (1H, s).

1. customPrecipitated crystals
2. customare separated through filtration
3. customdried