反应详情

温度

65 °C

N-(4-Bromo-3-fluoro-2-methylphenyl)acetamide (36 mmol) was suspended in 1,2 dichloroethane (150 mL) and acetic anhydride (108 mmol), potassium acetate (74 mmol), 18-Crown-6 (1.4 mmol) and isopentyl nitrite (79 mmol) were added sequentially. The mixture was heated at 65° C. for 24 h, cooled to rt and washed with sat. NaHCO3. The organic layer was dried (Na2SO4) and concentrated and the residue was purified by flash chromatography (0-20% EtOAc/hexanes). 1-(5-Bromo-4-fluoroindazol-1-yl)ethanone was obtained as a brown solid.

1. temperaturecooled to rt
2. washwashed with sat. NaHCO3
3. dry with materialThe organic layer was dried (Na2SO4)
4. concentrationconcentrated
5. customthe residue was purified by flash chromatography (0-20% EtOAc/hexanes)