反应详情

4.3 g (0.01 mol) of 11-[4-[2-[(diethylamino)methyl]-1-piperidinyl]-but-2-ynyl]-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one were dissolved in 40 ml of ethanol and after the addition of 0.5 g of 10% palladium on animal charcoal the mixture was hydrogenated under 3 bar of hydrogen pressure and at ambient temperature until the uptake of hydrogen had ceased. The mixture was filtered, the filtrate was evaporated down in a water jet vacuum and the oily residue remaining was purified by column chromatography on silica gel (Macherey-Nagel 60, 0.063-0.2 mm) using firstly ethyl acetate, then ethyl acetate/methanol/conc. ammonia 90/10/2 as eluant. From the fractions, after evaporation of the solvent and recrystallisation of the residue from diisopropyl ether, colourless crystals were obtained, m.p. 112° C., RF 0.75 (Merck, ready-made TLC plates, silica gel 60F-254; eluant: dichloromethane/cyclohexane/methanol/conc. ammonia 68/15/15/2 v/v/v/v). Yield: 2.2 g (50.5% of theory).

1. filtrationThe mixture was filtered
2. customthe filtrate was evaporated down in a water jet vacuum
3. customthe oily residue remaining was purified by column chromatography on silica gel (Macherey-Nagel 60, 0.063-0.2 mm)
4. customFrom the fractions, after evaporation of the solvent and recrystallisation of the residue from diisopropyl ether
5. customcolourless crystals were obtained