反应详情

温度

110 °C

A suspension of 4-fluoro-2-trifluoromethylbenzaldehyde (500 mg, 2.60 mmol), dimethylamine (5.5 mol/L in ethanol, 0.95 mL, 5.2 mmol), potassium carbonate (360 mg, 2.6 mmol) in 5.2 mL of N,N-dimethylformamide was stirred at 110° C. overnight in a sealed tube. After the reaction mixture was diluted with water, the solution was extracted with ether. The extract was washed with 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=85/15 to 75/25) to obtain the title compound as a pale yellow powder (393 mg, 70%).

1. extractionthe solution was extracted with ether
2. washThe extract was washed with brine
3. dry with materialdried over MgSO4
4. filtrationAfter filtration
5. concentrationthe filtrate was concentrated in vacuo
6. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=85/15 to 75/25)