反应详情

温度

80 °C

To a solution of methyl 3,5-dibromobenzoate (1 eq.) from the previous step in DMF (0.2 M) was added 2-[(1E)-3-methoxyprop-1-en-1-yl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (2.1 eq.), palladium acetate (10 mol %), triphenylphosphine (30 mol %), and 2.0 M aqueous sodium carbonate solution (5 eq.). The reaction was heated to 80° C. and stirred for 3 h. After cooling to rt, the reaction was diluted with ether. The organic extract was washed with water, brine, dried over MgSO4, and concentrated in vacuo. The crude product was purified by flash column chromatography (SiO2, 20% EtOAc in Hex) to afford the title compound as an oil.

1. temperatureAfter cooling to rt
2. extractionThe organic extract
3. washwas washed with water, brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by flash column chromatography (SiO2, 20% EtOAc in Hex)