反应详情

To 3-chloro[1,4]benzodioxino[2,3-c]pyridazine (1.71 g) was added a mixed solvent of dimethyl sulfoxide-methanol (1:1) (40 ml), and the mixture was stirred. 1,1′-Bis(diphenylphosphino)ferrocene (1.72 g), diacetoxypalladium (350 mg) and triethylamine (2.2 mL) were added, and the mixture was stirred under a carbon monoxide atmosphere at 1 atm, 80° C. for 19 hr. Water was added and the mixture was extracted with ethyl acetate, and the organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give methyl[1,4]benzodioxino[2,3-c]pyridazine-3-carboxylate (950 mg).

1. stirringthe mixture was stirred under a carbon monoxide atmosphere at 1 atm, 80° C. for 19 hr
2. extractionthe mixture was extracted with ethyl acetate
3. washthe organic layer was washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationThe solvent was concentrated under reduced pressure
6. customthe obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate)