تفاعل #586085
ord-bb154c89e28c4b1f8428b07c467ceca8
معادلة التفاعل
المتفاعلات
الكواشف
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المعالجة
- 1أخرىto settle leaving a colorless solution above it
- 2ترشيحThe reaction mixture was filtered once through a celite/acetone pad
- 3أخرىagain through a fritted glass funnel to remove the KCl
- 4أخرىThe acetone was removed in vacuo first on a rotovap
- 5workup.WAITon a high vacuum line (4 Pa, 25 degrees C.) for 2 hr
- 6أخرىResidual KCl was still precipitating out of the solution, so methylene chloride (50 ml)
- 7workup.ADDITIONwas added to the crude product, which
- 8غسيلwas then washed with deionized water (2×50 ml)
- 9تجفيفThe solution was dried over magnesium sulfate
- 10أخرىthe solvent was removed in vacuo
الإجراء التجريبي
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).