反应详情

A heterogeneous mixture of 4-(4-methylpiperazinyl)-3-methylnitrobenzene 5 (20 g, 85 mmol), 10% Pd/C (1.3 g) in methanol (1.2 liter) was hydrogenated [H2] at 40 PSI for 3 hours. The palladium catalyst was filtered through a pad of celite, washed with methanol (3×50 mL) and the combined filtrate was concentrated to afford 4-(4-methylpiperazin-1-yl)-3-methylaniline 7 (15 g, 86%). 1H NMR (CD3OD): δ6.83 (d, 1H, J=8.7 Hz), 6.59 (d, 1H, J=2.7 Hz), 6.54 (dd, 1H, J=8.4 and 2.7 Hz), 2.84 (t,4H, J=4.8 Hz), 2.60 (bm,4H), 2.34 (s, 3H), 2.00 (s, 3H); LCMS: purity: 99.9%, MS (m/e): 206 (MH+).

1. customfor 3 hours
2. filtrationThe palladium catalyst was filtered through a pad of celite
3. washwashed with methanol (3×50 mL)
4. concentrationthe combined filtrate was concentrated