反应 #586085

ord-bb154c89e28c4b1f8428b07c467ceca8

反应方程式

[Cl-].[K+]
KCl
CCCC[n+]1ccn(C)c1.[Cl-]
1-Butyl-3-methylimidazolium chloride
O=S(=O)([O-])C(F)(F)C(F)OC(F)(F)C(F)(F)F.[K+]
potassium 1,1,2-trifluoro-2-(perfluoroethoxy)ethanesulfonate
CCCC[n+]1ccn(C)c1.O=S(=O)([O-])C(F)(F)C(F)OC(F)(F)C(F)(F)F
product
收率 62.0%
CCCC[n+]1ccn(C)c1.O=S(=O)([O-])C(F)(F)C(F)OC(F)(F)C(F)(F)F
1-butyl-3-methylimidazolium 1,1,2-trifluoro-2-(perfluoroethoxy)ethanesulfonate
收率 62.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他to settle leaving a colorless solution above it
  2. 2
    过滤The reaction mixture was filtered once through a celite/acetone pad
  3. 3
    其他again through a fritted glass funnel to remove the KCl
  4. 4
    其他The 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
    其他Residual 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
    洗涤was then washed with deionized water (2×50 ml)
  9. 9
    干燥The solution was dried over magnesium sulfate
  10. 10
    其他the solvent was removed in vacuo

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07765823B2uspto-grants-2010_08