反应详情

In an amount of 30.0 g (49 mmol) of 1,4-di(3,3,4,4,5,5,6,6,6-nonafluorohexyl) maleate, 6.8 mL (54 mmol) of N,N-dimethylaminopropylamine and 7.5 g (54 mmol) of potassium carbonate were dissolved in 120 mL of acetonitrile and refluxed for 6 hours with heating. Then, the reaction mixture was transferred to a separatory funnel and added with 1000 mL of ethyl acetate. The organic phase was washed with a saturated aqueous sodium hydrogencarbonate solution. Then, the organic layer was collected, and the organic solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=100:3 (volume ratio)) to obtain 2.64 g (yield: 75%) of the target compound as a brown oily compound.

1. temperaturerefluxed for 6 hours
2. temperaturewith heating
3. customThen, the reaction mixture was transferred to a separatory funnel
4. washThe organic phase was washed with a saturated aqueous sodium hydrogencarbonate solution
5. customThen, the organic layer was collected
6. customthe organic solvent was evaporated under reduced pressure
7. customThe residue was purified by silica gel column chromatography (chloroform:methanol=100:3 (volume ratio))