反应详情

温度

140 °C

To a solution of 4-fluorophenol (10 g, 89 mmol) and 4-fluorobenzaldehyde (11.07 g, 89 mmol) in DMF (200 mL) was added K2CO3 (13.33 g, 96 mmol). The mixture was heated at 140° C. for 4 h. After cooling to room temperature, the mixture was poured into of ice water (300 mL), and left stand overnight. The solid was collected by filtration, washed with water, re-dissolved in EA (200 mL) and washed with brine (100 mL). The organic phase was dried with sodium sulfate, filtered and concentrated to afford the title compound (17 g, 75 mmol, 84% yield) as yellow solid. LCMS: rt=1.52 min, [M+H+]=217

1. temperatureAfter cooling to room temperature
2. waitleft
3. filtrationThe solid was collected by filtration
4. washwashed with water
5. dissolutionre-dissolved in EA (200 mL)
6. washwashed with brine (100 mL)
7. dry with materialThe organic phase was dried with sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated