반응 #586085

반응 방정식

KCl

1-Butyl-3-methylimidazolium chloride

potassium 1,1,2-trifluoro-2-(perfluoroethoxy)ethanesulfonate

→

product

수율 62.0%

1-butyl-3-methylimidazolium 1,1,2-trifluoro-2-(perfluoroethoxy)ethanesulfonate

수율 62.0%

용매

acetone

acetone

반응 조건

후처리

1. 1
   기타to settle leaving a colorless solution above it
2. 2
   여과The reaction mixture was filtered once through a celite/acetone pad
3. 3
   기타again through a fritted glass funnel to remove the KCl
4. 4
   기타The acetone was removed in vacuo first on a rotovap
5. 5
   workup.WAITon a high vacuum line (4 Pa, 25 degrees C.) for 2 hr
6. 6
   기타Residual KCl was still precipitating out of the solution, so methylene chloride (50 ml)
7. 7
   workup.ADDITIONwas added to the crude product, which
8. 8
   세척was then washed with deionized water (2×50 ml)
9. 9
   건조The solution was dried over magnesium sulfate
10. 10
    기타the solvent was removed in vacuo

실험 절차

1-Butyl-3-methylimidazolium chloride (Bmim-Cl, 7.8 g) and dry acetone (150 ml) were combined at room temperature in a 500 ml flask. At room temperature in a separate 200 ml flask, potassium 1,1,2-trifluoro-2-(perfluoroethoxy)ethanesulfonate (TPES-K, 15.0 g) was dissolved in dry acetone (300 ml). These two solutions were combined and allowed to stir magnetically for 12 hr under positive nitrogen pressure. The KCl precipitate was then allowed to settle leaving a colorless solution above it. The reaction mixture was filtered once through a celite/acetone pad and again through a fritted glass funnel to remove the KCl. The acetone was removed in vacuo first on a rotovap and then on a high vacuum line (4 Pa, 25 degrees C.) for 2 hr. Residual KCl was still precipitating out of the solution, so methylene chloride (50 ml) was added to the crude product, which was then washed with deionized water (2×50 ml). The solution was dried over magnesium sulfate, and the solvent was removed in vacuo to give the product as a viscous light yellow oil (12.0 g, 62% yield).

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