反应详情

温度

75 °C

To a solution of methyl 2-methoxy-4-trifluoromethanesulfonyloxybenzoate (26.8 g), t-butyl acrylate (62.5 ml), triethylamine (25 ml) in anhydrous dimethylformamide (100 ml) are added palladium acetate (0.4 g) and 1,3-bis(diphenylphosphino)propane (0.74 g) under argon atmosphere, and the mixture is heated with stirring at 75° C. for 16 hours. The reaction solution is concentrated under reduced pressure to remove the solvent, and thereto is added water. The mixture is extracted with ethyl acetate, and the extract is washed with water, dried, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (solvent; ethyl acetate:n-hexane=1:5) to give t-butyl 3-methoxy-4-methoxycarbonylcinnamate (23.5 g).

1. temperaturethe mixture is heated
2. concentrationThe reaction solution is concentrated under reduced pressure
3. customto remove the solvent
4. additionis added water
5. extractionThe mixture is extracted with ethyl acetate
6. washthe extract is washed with water
7. customdried
8. concentrationconcentrated under reduced pressure
9. customThe residue is purified by silica gel column chromatography (solvent; ethyl acetate:n-hexane=1:5)