反应详情

Mono(2-ethylhexyl)mono(2,2,3,3,4,4,4-heptafluorobutyl)maleate (80.3 g, 0.196 mol), sodium hydrogensulfite (20.4 g, 0.196 mol) and water/ethanol (80 mL, 1:1 (v/v)) were mixed and refluxed for 10 hours with heating. Then, the reaction mixture was added with ethyl acetate (1000 mL), and the organic phase was washed with saturated sodium chloride aqueous solution. Thereafter, 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=9/1 (v/v)). The corrected organic phase was washed with a saturated sodium chloride aqueous solution, and then the organic solvent was evaporated under reduced pressure to obtain the target compound (32 g, yield: 32%) as colorless transparent solid.

1. temperaturerefluxed for 10 hours
2. temperaturewith heating
3. washthe organic phase was washed with saturated sodium chloride aqueous solution
4. customThereafter, the organic layer was collected
5. customthe organic solvent was evaporated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (chloroform/methanol=9/1 (v/v))
7. washThe corrected organic phase was washed with a saturated sodium chloride aqueous solution
8. customthe organic solvent was evaporated under reduced pressure