反应详情

温度

40 °C

To a solution of compound 3 ethyl 4-fluoro-3-vinylbenzoate (Preparation 54, 87 g, 0.42 mol, 1 eq) in THF (470 mL) and water (400 mL) was added lithium hydroxide monohydrate (35.1 g, 0.84 mol, 2.0 eq). The resulting mixture was stirred at 40° C. overnight. THF was removed in vacuum, then 6N hydrogen chloride solution was added dropwise until pH=2. The mixture was extracted with ethyl acetate (3×600 mL). The organic phase was dried over sodium sulfate and concentrated in vacuo to give title compound as a white solid (60.8 g, 0.34 mol, 81%).

1. customTHF was removed in vacuum
2. addition6N hydrogen chloride solution was added dropwise until pH=2
3. extractionThe mixture was extracted with ethyl acetate (3×600 mL)
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated in vacuo