反应详情

温度

85 °C

A mixture of 1,2-dibromo-3,5-difluorobenzene (24.7 g, 91.6 mmol), bis(triphenylphosphine)palladium(II) chloride (2.57 g, 3.66 mmol) and triethylamine (51.0 mL, 366 mmol) in 300 mL of DMF was stirred under argon at approximately 85° C. for 15 minutes. Hydrazine hydrate (366 μL, 7.54 mmol) was added and the mixture was stirred for an additional 10 minutes. Ethyl acrylate (39.7 mL, 366 mmol) was added and the mixture was stirred under argon at approximately 85° C. for approximately 144 hours. The solvents were removed by evaporation under reduced pressure and the residue was dissolved in 1.0 L of ethyl acetate. The ethyl acetate solution was washed 3 times with water and dried over magnesium sulfate. Evaporation of the solvent gave crude ethyl 3-{3,5-difluoro-2-[2-(ethoxycarbonyl)vinyl]phenyl}acrylate (36 g).

1. stirringthe mixture was stirred for an additional 10 minutes
2. stirringthe mixture was stirred under argon at approximately 85° C. for approximately 144 hours
3. customThe solvents were removed by evaporation under reduced pressure
4. dissolutionthe residue was dissolved in 1.0 L of ethyl acetate
5. washThe ethyl acetate solution was washed 3 times with water
6. dry with materialdried over magnesium sulfate
7. customEvaporation of the solvent