反应详情

温度

110 °C

To a solution of (E)-1-(2-bromo-4-methoxyphenyl)-3-phenyl-2-propen-1-one (6.0 g, 18.91 mmol) obtained in Step 2 in DMF (15 mL) was added PPh3 (1.46 g, 5.68 mmol, 0.3 eq), K2CO3 (5.23 g, 37.83 mmol, 2 eq), and PdCl2 (335 mg, 1.89 mmol, 0.1 eq). The reaction vial was heated to 110° C. for 3 h. After cooling to room temperature, the reaction mixture was diluted with EtOAc and filtered through a Celite pad. The solution was washed with H2O and brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexanes=1:5) to afford the desired product (2.8 g, 63%).

1. customThe reaction
2. temperatureAfter cooling to room temperature
3. filtrationfiltered through a Celite pad
4. washThe solution was washed with H2O and brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by silica gel column chromatography (EtOAc/hexanes=1:5)