反应详情

温度

50 °C

Sodium carbonate (19.50 g, 0.184 mol) was dispersed into a solution of 2,3,4-trifluorophenol (13.64 g, 0.092 mol) in acetone (300 mL). To the stirred suspension was added the solution of benzyl bromide (17.31 g, 101.21 mmol) in acetone (100 mL) dropwisely. The mixture was heated under reflux at 50° C. for 24 h, allowed to cool to room temperature, and filtered. The filter cake was washed with acetone (50 mL×3), and acetone was removed under reduced pressure. The residue was dissolved in ethyl acetate (500 mL). The solution was washed with 5% sodium hydroxide (50 mL), water (150 mL) and brine (150 mL) sequentially and dried over Na2SO4. The solvent was removed in vacuo to yield a pale yellow solid (19.89 g, 90% yield). 1H NMR (400 MHz, CDCl3): δ 7.40 (m, 5H), 6.85 (m, 1H), 6.64 (m, 1H), 5.15 (s, 2H).

1. temperatureThe mixture was heated
2. temperatureto cool to room temperature
3. filtrationfiltered
4. washThe filter cake was washed with acetone (50 mL×3), and acetone
5. customwas removed under reduced pressure
6. dissolutionThe residue was dissolved in ethyl acetate (500 mL)
7. washThe solution was washed with 5% sodium hydroxide (50 mL), water (150 mL) and brine (150 mL) sequentially
8. dry with materialdried over Na2SO4
9. customThe solvent was removed in vacuo