反应详情

To a solution of ethyl-3-(5′-fluoro-2′-methoxyphenyl)acrylate (6.0 g, 27 mmol) in ethanol (100%, 80 mL) under Ar was added Pd/C (10%, 250 mg) very carefully and the flask containing the mixture was evacuated and purged with H2 three time each. Then a H2 balloon was attached to the flask and charged with H2 and the reaction was allowed to go for 20 h at room temperature. Then the reaction mixture was filtered through a pad of silica eluted with mixed solvent of EtOAc and Hexane (1:1). The crude product that obtained by removal of the solvent in vacuo was purified by flash column chromatography (10% EtOAc in hexane, Rf=0.20) to give the product (5.8 g, 95%).

1. additionthe flask containing the mixture
2. customwas evacuated
3. custompurged with H2 three time each
4. additioncharged with H2
5. filtrationThen the reaction mixture was filtered through a pad of silica
6. washeluted with mixed solvent of EtOAc and Hexane (1:1)
7. customThe crude product that obtained by removal of the solvent in vacuo
8. customwas purified by flash column chromatography (10% EtOAc in hexane, Rf=0.20)