反应详情

14.6 g of 2,2,3,3,4,4,5,5-octafluoropentyl trifluoromethanesulfonate was dissolved in 30 ml of dimethyl sulfoxide, and 5.5 g of potassium carbonate was added. Further, 2.6 g of malononitrile dissolved in 10 ml of dimethyl sulfoxide was added dropwise, and the mixture was stirred at room temperature for 3 hours. Further, 7.0 g of 2,2,3,3,4,4,5,5-octafluoropentyl trifluoromethanesulfonate and 2.7 g of potassium carbonate were added, and the mixture was stirred for 1 hour. Thereafter, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed successively with water and aqueous saturated sodium chloride, dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography. The resulting fraction was concentrated and washed with chloroform to obtain 0.13 g of 2,2-bis(2,2,3,3,4,4,5,5-octafluoropentyl)malononitrile (hereinafter, referred to as the present compound (49)).

1. additionwas added dropwise
2. stirringthe mixture was stirred for 1 hour
3. extractionfollowed by extraction with ethyl acetate
4. washThe organic layer was washed successively with water and aqueous saturated sodium chloride
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. concentrationThe resulting fraction was concentrated
8. washwashed with chloroform