反応 #1106617

ord-59adb1bea6894374bb1d576fc785a7bb

反応方程式

[Cl-].[K+]
KCl
O=S(=O)([O-])C(F)(F)C(F)F.[K+]
potassium 1,1,2,2-tetrafluoroethanesulfonate
CC[n+]1ccn(C)c1.[Cl-]
1-ethyl-3methylimidazolium chloride
CC[n+]1ccn(C)c1.[Cl-]
Emim-Cl
CC[n+]1ccn(C)c1.O=S(=O)([O-])C(F)(F)C(F)F
oil
収率 64.0%
CC[n+]1ccn(C)c1.O=S(=O)([O-])C(F)(F)C(F)F
1-ethyl-3-methylimidazolium 1,1,2,2-tetrafluoroethane sulfonate
収率 64.0%

反応条件

温度
24°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISSOLUTIONdissolved
  2. 2
    その他These solutions were combined in a 1 l flask
  3. 3
    その他producing a milky white suspension
  4. 4
    workup.STIRRINGThe mixture was stirred at 24 degrees C
  5. 5
    その他to settle leaving a clear green solution above it
  6. 6
    ろ過The reaction mixture was filtered once through a celite/acetone pad and again through a fritted glass funnel
  7. 7
    その他to remove the KCl
  8. 8
    その他The acetone was removed in vacuo first on a rotovap
  9. 9
    workup.WAITon a high vacuum line (4 Pa, 25 degrees C.) for 2 hr

実験手順

To a 500 ml round bottom flask was added 1-ethyl-3methylimidazolium chloride (Emim-Cl, 98%, 61.0 g) and reagent grade acetone (500 ml). The mixture was gently warmed (50 degrees C.) until almost all of the Emim-Cl dissolved. To a separate 500 ml flask was added potassium 1,1,2,2-tetrafluoroethanesulfonate (TFES-K, 90.2 g) along with reagent grade acetone (350 ml). This second mixture was stirred magnetically at 24 degrees C. until all of the TFES-K dissolved. These solutions were combined in a 1 l flask producing a milky white suspension. The mixture was stirred at 24 degrees C. for 24 hrs. The KCl precipitate was then allowed to settle leaving a clear green 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. The product was a viscous light yellow oil (76.0 g, 64% yield).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08715521B2uspto-grants-2014_05