反应详情

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).

1. customto settle leaving a colorless solution above it
2. filtrationThe reaction mixture was filtered once through a celite/acetone pad
3. customagain through a fritted glass funnel to remove the KCl
4. customThe acetone was removed in vacuo first on a rotovap
5. waiton a high vacuum line (4 Pa, 25 degrees C.) for 2 hr
6. customResidual KCl was still precipitating out of the solution, so methylene chloride (50 ml)
7. additionwas added to the crude product, which
8. washwas then washed with deionized water (2×50 ml)
9. dry with materialThe solution was dried over magnesium sulfate
10. customthe solvent was removed in vacuo