反应详情

To a mixture of ethyl 4-fluoro-3-vinylbenzoate (Preparation 54, 48 g, 0.25 mol, 1 eq) and palladium (II) acetate (2.5 g, 10 mmol, 0.4 eq) in ether (300 mL) was added diazomethane in ether (1.5 mol, 6.0 eq). Then the mixture was stirred at room temperature overnight. The reaction was quenched with a solution of AcOH (75 mL) in water (100 mL). The mixture was filtrated and the filtrate was added saturated solution of sodium carbonate until pH=10. The organic phase was washed with brine (200 mL) and water (200 mL), dried over sodium sulfate and concentrated in vacuo to give title compound as brown liquid (51 g, 0.248 mol, 99.1%).

1. customThe reaction was quenched with a solution of AcOH (75 mL) in water (100 mL)
2. filtrationThe mixture was filtrated
3. additionthe filtrate was added saturated solution of sodium carbonate until pH=10
4. washThe organic phase was washed with brine (200 mL) and water (200 mL)
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated in vacuo