反应详情

In DMF (2 ml) was dissolved 3,5-dimethyl-1H-pyrazolo [3,4-d]pyridazin-4(5H)-one (94 mg) followed by addition of 4-(4-chlorobenzoyl)benzyl bromide (279 mg) and potassium carbonate (124 mg), and the mixture was stirred at room temperature for 15 hours. This reaction mixture was extracted with ethyl acetate and the organic layer was serially washed with water and saturated aqueous NaCl solution, dried over anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (n-hexane: ethyl acetate=1:4), washed with the following solvent, and dried. As the washing solvent, n-hexanediethyl ether was used for 1-[4-(4-chlorobenzoyl) benzyl]-3,5-dimethyl-1H-pyrazolo[3,4-d]pyridazin-4(5H)-one and diethyl ether for 2-[4-(4-chlorobenzoyl)benzyl]-3,5-dimethyl-2H-pyrazolo [3,4-d]pyridazin-4(5H)-one.

1. extractionThis reaction mixture was extracted with ethyl acetate
2. washthe organic layer was serially washed with water and saturated aqueous NaCl solution
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography (n-hexane: ethyl acetate=1:4)
6. washwashed with the following solvent
7. customdried