反应详情

9.38 g (40.2 mmol) of 3-(5-Bromo-thiophen-2-yl)-acrylic acid and 6.97 g (6 mmol) of tetrakis(triphenylphosphine)palladium were dissolved in 50 ml of degassed DME and stirred for 10 min at room temperature. 8.44 g (60.4 mmol) of 2-fluorophenylboronic acid and 50 ml of a 2 M aqueous sodium carbonate solution were added together with an additional 5 ml of degassed DME. The reaction mixture was heated to 95° C. for 4 h, and then stirred at room temperature for 16 h. The product precipitated partially from the reaction solution and was collected by filtration. This solid was boiled for 1 h in ethyl acetate and filtered while hot. The solvent was removed under reduced pressure. The remaining reaction solution was evaporated to dryness. The residue was taken up in ethyl acetate/water and filtered. The organic phase was dried with sodium sulfate, filtered and the solvent was removed under reduced pressure. The combined product was purified by silica gel chromatography. Yield: 7.5 g.

1. temperatureThe reaction mixture was heated to 95° C. for 4 h
2. stirringstirred at room temperature for 16 h
3. customThe product precipitated partially from the reaction solution
4. filtrationwas collected by filtration
5. waitThis solid was boiled for 1 h in ethyl acetate
6. filtrationfiltered while hot
7. customThe solvent was removed under reduced pressure
8. customThe remaining reaction solution
9. customwas evaporated to dryness
10. filtrationfiltered
11. dry with materialThe organic phase was dried with sodium sulfate
12. filtrationfiltered
13. customthe solvent was removed under reduced pressure
14. customThe combined product was purified by silica gel chromatography