反应详情

In DMF (10 ml) was dissolved 5-t-butyl-3-methyl-1H-pyrazolo [3,4-d]pyridazin-4(5H)-one (516 mg) followed by addition of 4-(4-fluorobenzoyl)benzyl bromide (1.1 g) and potassium carbonate (525 mg), and the mixture was stirred at room temperature for 15 hours. This reaction mixture was extracted with diethyl ether 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-hexaneethyl acetate=1:1), washed with the following solvent, and dried. As the washing solvent, n-hexanediethyl ether was used for 5-t-butyl-1-[4-(4-fluorobenzoyl) benzyl]-3-methyl-1H-pyrazolo[3,4-d]-pyridazin-4(5H)-one and diethyl ether-ethyl acetate for 5-t-butyl-2-[4-(4-fluorobenzoyl)benzyl]-3-methyl-2H-pyrazolo [3,4-d]pyridazin-4(5H)-one.

1. extractionThis reaction mixture was extracted with diethyl ether
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-hexaneethyl acetate=1:1)
6. washwashed with the following solvent
7. customdried