反应详情

To a mixture of 4-chloro-2-methyl-5-(4-methylpiperazin-1-yl)pyridazin-3(2H)-one (4.85 g, 20 mmol) and 10% Pd/C catalyst (1.14 g) in methanol (100 ml) was added ammonium formate (2.90 g, 46 mmol), and the mixture was refluxed under argon with TLC monitoring (dichloromethane:methanol (9:1)). Further portions of ammonium formate were added until the starting material was completely consumed. The catalyst was filtered off and washed with methanol, then the solvent was evaporated under reduced pressure. The residue was taken up in water (30 ml) and extracted with dichloromethane (4×40 ml). The combined extracts were washed with water, dried (Na2SO4) and evaporated. The crude product was purified by recrystallization from ethyl acetate:light petroleum.

1. customwas completely consumed
2. filtrationThe catalyst was filtered off
3. washwashed with methanol
4. customthe solvent was evaporated under reduced pressure
5. extractionextracted with dichloromethane (4×40 ml)
6. washThe combined extracts were washed with water
7. dry with materialdried (Na2SO4)
8. customevaporated
9. customThe crude product was purified by recrystallization from ethyl acetate