反应详情

0.250 g (1.1 mmol) of 3-(5-bromo-thiophen-2-yl)-acrylic acid and 61.9 mg (0.1 mmol) of tetrakis(triphenylphosphine)palladium were dissolved in 5 ml of degassed DME and stirred at room temperature for 10 min. 0.251 g (1.6 mmol) of 4-chlorophenylboronic acid and 1 ml of a 2 M aqueous sodium carbonate solution were added together with an additional 5 ml of degassed DME. The resulting solution was heated to 95° C. for 4 h and then stirred at room temperature for 16 h. Solids were removed by filtration, and the resulting solution was evaporated to dryness. The residue was dissolved in ethyl acetate and washed three times with a saturated sodium hydrogencarbonate solution and once with a saturated sodium chloride solution. The organic phase was dried with sodium sulfate, filtered, and the solvent was removed under reduced pressure. The product was purified by silica gel chromatography. Yield: 0.12 g.

1. temperatureThe resulting solution was heated to 95° C. for 4 h
2. stirringstirred at room temperature for 16 h
3. customSolids were removed by filtration
4. customthe resulting solution was evaporated to dryness
5. dissolutionThe residue was dissolved in ethyl acetate
6. washwashed three times with a saturated sodium hydrogencarbonate solution
7. dry with materialThe organic phase was dried with sodium sulfate
8. filtrationfiltered
9. customthe solvent was removed under reduced pressure
10. customThe product was purified by silica gel chromatography