반응 #53247

반응 방정식

Potassium perfluorobutanesulfonate

2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide

→

2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate

수율 64.2%

용매

water

methanol

methanol

반응 조건

후처리

1. 1
   기타a solution obtained
2. 2
   workup.ADDITIONwas added to the above solution
3. 3
   추출The aqueous solution was extracted twice with 100 ml of chloroform
4. 4
   세척the organic phase was washed with water
5. 5
   농축concentrated
6. 6
   기타an oily product was obtained
7. 7
   농축The above-obtained product was concentrated again with ethyl acetate
8. 8
   기타a solid product was obtained
9. 9
   여과The solid product was filtered and re-slurried with diisopropyl ether

실험 절차

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.

출처