Methanol → HCID 10172811, compound

Participants

Reaction Steps

Into a pressure-tight hydrogenating apparatus 1.64 g (0.0039 mole) of 5-{2-[4-(6-fluoro-1,2-benzisoxazole-3-yl)-piperidine-1-yl]-propylamino}-4-chloro2-methyl-2H-pyridazine-3-one, 150 ml of a solvent mixture (9:1 mixture of methanol and distilled water), 0.18 g (0.0456 mole) of sodium hydroxide and 3.2 g of a palladium/charcoal catalyst (composition: 8% of palladium, 28% of carbon and 64% of water) are weighed in. The reaction mixture is stirred at a hydrogen pressure of 10 atm. for 24 hours. The reaction mixture is heated to reflux temperature and stirred at this temperature for 5 minutes. The mixture is filtered hot and the catalyst is washed five times with 33 ml of a 1:1 mixture of methanol and dichloro methane each. The united mother lyes are evaporated. The precipitated crude product is recrystallized from a mixture of acetonitrile and water. Thus 1.12 g of the desired compound are obtained. Yield 73.8%.

Provenance & Evidence