反应详情

2-Cyano-N-(4-methoxy-3-pyridyl)acetamide 8 (26.4 g, 138.1 mmol) was slurried in ethanol (300 mL). Sodium acetate (23.56 g, 287.2 mmol) was added followed by trichloroacetonitrile (23.92 g, 16.85 mL, 165.7 mmol). The mixture was stirred at room temperature overnight. The suspension was filtered and the solids washed with ethanol. The solids (46.5 g) were slurried for 90 minutes in 10% aqueous ethanol, filtered and dried to afford 3-amino-4,4,4-trichloro-2-cyano-N-(4-methoxy-3-pyridyl)but-2-enamide (37.2 g, 80%). LC-MS (M+H)+ 336.9; 1H NMR (500 MHz, DMSO-d6) δ 8.44 (d, 1H), 7.43-7.47 (m, 1H), 6.35-6.39 (m, 1H), 4.04 (s, 3H).

1. filtrationThe suspension was filtered
2. washthe solids washed with ethanol
3. waitThe solids (46.5 g) were slurried for 90 minutes in 10% aqueous ethanol
4. filtrationfiltered
5. customdried