反应详情

Raney nickel (0.55 g) was added to a mixture of 4-[amino[4-(3-chlorophenyl)-1,2-dihydro-1-methyl-2-oxo-6-quinolinyl](1-methyl-1H-imidazol-5-yl)methyl]-benzonitrile, (0.0011 mol) in CH3OH/NH3 7N (12 ml) under N2 flow. The mixture was hydrogenated overnight under a 5 bar pressure, then filtered over celite. The filtrate was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 92/8/0.5; 15–40 μm). The pure fractions were collected and the solvent was evaporated, yielding 0.36 g (65%)g of 6-[amino[4-(aminomethyl)phenyl](1-methyl-1H-imidazol-5-yl)methyl]-4-(3-chlorophenyl)-1-methyl-2(1H)-quinolinone, mp. 150° C.

1. filtrationfiltered over celite
2. customThe filtrate was evaporated
3. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 92/8/0.5; 15–40 μm)
4. customThe pure fractions were collected
5. customthe solvent was evaporated