反应详情

温度

-60 °C

14.0 g (48.0 mmol) of 6,6′-(1-(pyridin-2-yl)ethane-1,1-diyl)bis(2-fluoropyridin) were dissolved in 300 ml of tetrahydrofurane and cooled to −60° C. 200 ml (100 mmol) of potassium diphenylphosphide (0.5 M solution in tetrahydrofurane) were added and the mixture was stirred for three days at room temperature. The reaction was hydrolysed with 200 ml of saturated ammonium chloride solution. The aqueous layer was extracted three times with ethyl acetate. The combined organic layers were washed two times with saturated ammonium chloride solution and dried with sodium sulphate. The solvent was removed under reduced pressure to yield 40 g (>100%) of crude product which was used in the next synthesis without further purification.

1. extractionThe aqueous layer was extracted three times with ethyl acetate
2. washThe combined organic layers were washed two times with saturated ammonium chloride solution
3. dry with materialdried with sodium sulphate
4. customThe solvent was removed under reduced pressure