Reaction #53247

Reaction equation

Potassium perfluorobutanesulfonate

2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide

→

2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate

Yield 64.2%

Solvents

water

methanol

methanol

Conditions

Workup

1. 1
   Othera solution obtained
2. 2
   workup.ADDITIONwas added to the above solution
3. 3
   ExtractionThe aqueous solution was extracted twice with 100 ml of chloroform
4. 4
   Washthe organic phase was washed with water
5. 5
   Concentrationconcentrated
6. 6
   Otheran oily product was obtained
7. 7
   ConcentrationThe above-obtained product was concentrated again with ethyl acetate
8. 8
   Othera solid product was obtained
9. 9
   FiltrationThe solid product was filtered and re-slurried with diisopropyl ether

Procedure

Potassium perfluorobutanesulfonate (10 g) was dissolved in a mixed solvent comprising 500 ml of water and 100 ml of methanol, and a solution obtained by dissolving 7.7 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide in 50 ml of methanol was added to the above solution. The aqueous solution was extracted twice with 100 ml of chloroform, the organic phase was washed with water and concentrated, thereby an oily product was obtained. The above-obtained product was concentrated again with ethyl acetate, thereby a solid product was obtained. The solid product was filtered and re-slurried with diisopropyl ether, to thereby obtain 9 g of 2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate.

Source