反应详情

80.3 g (0.196 mol) of mono(2-ethylhexyl)mono(2,2,3,3,4,4,4-heptafluorobutyl)maleate, 20.4 g (0.196 mol) of sodium hydrogen sulfite and 80 mL of water/ethanol (1/1 v/v) were mixed together and heated under reflux for 10 hr. Thereafter, 1000 mL of ethyl acetate was added, and the organic phase was washed with a saturated aqueous sodium chloride solution. The resultant organic layer was collected, and the organic solvent was distilled off in vacuum. Purification by silica gel column chromatography (chloroform/methanol: 9/1 v/v) was performed. The collected organic phase was washed with a saturated aqueous sodium chloride solution, and the organic solvent was distilled off in vacuum, thereby obtaining 32 g (yield: 32%) of desired compound as a colorless transparent solid.

1. temperatureheated
2. temperatureunder reflux for 10 hr
3. washthe organic phase was washed with a saturated aqueous sodium chloride solution
4. customThe resultant organic layer was collected
5. distillationthe organic solvent was distilled off in vacuum
6. customPurification by silica gel column chromatography (chloroform/methanol: 9/1 v/v)
7. washThe collected organic phase was washed with a saturated aqueous sodium chloride solution
8. distillationthe organic solvent was distilled off in vacuum