反应详情

温度

130 °C

A suspension of 9.72 g (4-bromo-3-fluoro-phenyl)-carbamic acid benzyl ester (30 mmol), 6 g ethyl acrylate (60 mmol), 10.2 ml DIPEA (60 mmol), 112 mg palladium acetate (, 3 mmol), and 1.57 g triphenylphosphine (6 mmol) in 10 ml DMF were stirred at 130° C. for 48 h. The reaction was monitored by TLC. The DMF was evaporated, the residue dissolved in dichloromethane, washed with water and brine, dried over Mg sulfate, filtered and the filtrate evaporated. The residue was purified by chromatography, using a 7/3 N-hexane/ethyl acetate mixture as eluent.

1. customThe DMF was evaporated
2. dissolutionthe residue dissolved in dichloromethane
3. washwashed with water and brine
4. dry with materialdried over Mg sulfate
5. filtrationfiltered
6. customthe filtrate evaporated
7. customThe residue was purified by chromatography