反应详情

温度

110 °C

To a suspension of 2-fluorobenzaldehyde (250 μL, 2.37 mmol) and potassium carbonate (328 mg, 2.37 mmol) in 5 mL of dry N,N-dimethylformamide was added dimethylamine/ethanol solution (0.65 mL, 5.6 M, 3.6 mmol) at room temperature. After being stirred at 110° C. for 12 h, the reaction mixture was diluted with ethyl acetate. The solution was washed with water, saturated NaHCO3 aqueous solution, brine, and dried over MgSO4. After filtration, the filtrate was concentrated in vacuo, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=90/10 to 80/20) to obtain the title compound as a yellow oil (299 mg, 85%).

1. washThe solution was washed with water, saturated NaHCO3 aqueous solution, brine
2. dry with materialdried over MgSO4
3. filtrationAfter filtration
4. concentrationthe filtrate was concentrated in vacuo
5. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=90/10 to 80/20)