反应详情

A solution of 2-fluoro-4-bromophenol 14-1 (50 g, 261.8 mmol), ethyl acrylate (34 mL), Pd(OAc)2 (2.5 g), tri-o-tolylphosphine (5 g) and triethylamine (83 mL) was heated to 100° C. in a sealed tube for 12 h. The reaction was cooled to room temperature and diluted with dichloromethane (100 mL). The organic solution was washed with 10% aq. citric acid (40 mL), satd aq NaHCO3, and brine (40 mL). The organic solution was dried over MgSO4, filtered and concentrated. The residue was purified by flash chromatography (50:50 hexanes/EtOAc to 100% EtOAc) to give acrylic acid 14-2 as a white solid.

1. washThe organic solution was washed with 10% aq. citric acid (40 mL)
2. dry with materialThe organic solution was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by flash chromatography (50:50 hexanes/EtOAc to 100% EtOAc)