反应详情

2-Amino-4-chloro-N-{3-methoxy-4-[2-(1-pyrrolidinyl)ethoxy]phenyl}benzamide (11.6 mmol, 4.5 g) was dissolved in 90 mL 88% formic acid and was heated to reflux for 3 h. The solvents were removed by rotary evaporation and the residue was purified by silica gel column chromatography affording the lo product (4.2 g, 91%). 1H NMR (DMSO-D6): δ 1.82 (4H, m), 2.65 (4H, m), 2.88 (2H, t, J=6.2 Hz), 3.88 (3H, s), 4.20 (2H, t, J=6.4 Hz), 6.89-6.91 (2H, overlapping), 7.01 (1H, d, J=10.1 Hz), 7.49 (1H, d, J=8.6 Hz), 7.76 (1H, s), 8.12 (1H, s), 8.29 (1H, d, 8.7 Hz). LCMS m/z=400 (m+H+).

1. temperaturewas heated
2. temperatureto reflux for 3 h
3. customThe solvents were removed by rotary evaporation
4. customthe residue was purified by silica gel column chromatography