反应详情

A mixture of N-(4-cyano-2-methyl-6-nitro-phenyl)-2,2,2-trifluoro-acetamide (5 g, 18.3 mmol) and 2 M ammonia in methanol (80 mL) was heated to reflux for 14 h and then cooled to room temperature. After concentration in vacuo, the residue was purified by flash chromatography (20% EtOAc/hexane) to yield the title compound (3.24 g, 100%, ca 80% pure). 1H NMR (300 MHz, CDCl3) δ 8.40 (1H, s), 7.47 (1H, s), 6.6–6.8 (2H, broad s), 2.89 (3H, s).

1. temperaturewas heated
2. temperatureto reflux for 14 h
3. concentrationAfter concentration in vacuo
4. customthe residue was purified by flash chromatography (20% EtOAc/hexane)