反应详情

温度

80 °C

125 mg (0.18 mmol) of bis(triphenylphosphine)palladium(II) chloride are added to a solution of 1 g (3.58 mmol) of 5-cyano-2-formylphenyl trifluoromethanesulfonate and 1.15 ml (3.94 mmol) of tri-n-butylvinylstannane in 6 ml of anhydrous and degassed DMF under an argon atmosphere. The reaction mixture is then stirred at 80° C. for 90 min Subsequently, 100 ml of 10% strength potassium fluoride solution are added, and the mixture is stirred at RT for 1 h. The suspension is extracted three times with 20 ml of ethyl acetate each time, and the combined organic phases are washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution. The organic solution is dried over magnesium sulfate and concentrated. The residue (0.6 g) is employed without further purification in the next stage.

1. customdegassed DMF under an argon atmosphere
2. addition100 ml of 10% strength potassium fluoride solution are added
3. stirringthe mixture is stirred at RT for 1 h
4. extractionThe suspension is extracted three times with 20 ml of ethyl acetate each time
5. washthe combined organic phases are washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution
6. dry with materialThe organic solution is dried over magnesium sulfate
7. concentrationconcentrated
8. customThe residue (0.6 g) is employed without further purification in the next stage