反应 #53247

反应方程式

Potassium perfluorobutanesulfonate

2-oxo-3,3-dimethylbutyltetrahydrothiophenium bromide

→

2-oxo-3,3-dimethylbutyltetrahydrothiophenium perfluorobutanesulfonate

收率 64.2%

溶剂

water

methanol

methanol

反应条件

后处理

1. 1
   其他a solution obtained
2. 2
   workup.ADDITIONwas added to the above solution
3. 3
   萃取The aqueous solution was extracted twice with 100 ml of chloroform
4. 4
   洗涤the organic phase was washed with water
5. 5
   浓缩concentrated
6. 6
   其他an oily product was obtained
7. 7
   浓缩The above-obtained product was concentrated again with ethyl acetate
8. 8
   其他a solid product was obtained
9. 9
   过滤The solid product was filtered and re-slurried with diisopropyl ether

实验过程

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.

来源