反应详情

2.5 g (6.3 mmol) of 6-[3-nitro-4[4-(2-pyrimidyl)-piperazin-1-yl]-phenyl]-4,5-dihydro-5-methyl-3(2H)-pyridazinone in 130 ml of methanol are hydrogenated under a hydrogen pressure of 5 bar in the presence of 0.3 g of palladium on active charcoal (10% Pd) at 50° C. for 3 hours. After removal of the catalyst by suction filtration, the filtrate is highly concentrated by evaporation under vacuum and the residue obtained is chromatographed on silica gel, using dichloromethane/methanol (95:5) as solvent. After concentration of the product fractions by evaporation, the residue obtained is crystallized with acetone. 0.70 g (30%) of pale beige crystals, m.p. 220° to 221° C., are obtained.

1. customat 50° C.
2. customfor 3 hours
3. customAfter removal of the catalyst
4. filtrationby suction filtration
5. concentrationthe filtrate is highly concentrated by evaporation under vacuum
6. customthe residue obtained
7. customis chromatographed on silica gel
8. customAfter concentration of the product fractions by evaporation
9. customthe residue obtained
10. customis crystallized with acetone