反応 #586084

ord-4e2a166ee5ed44bdaa0711513c41caba

反応方程式

CCCC[n+]1ccn(C)c1.[Cl-]
1-Butyl-3-methylimidazolium chloride
O=S(=O)([O-])C(F)(F)C(F)OC(F)(F)F.[K+]
potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonate
CCCC[n+]1ccn(C)c1.O=S(=O)([O-])C(F)(F)C(F)OC(F)(F)F
product
収率 67.8%
CCCC[n+]1ccn(C)c1.O=S(=O)([O-])C(F)(F)C(F)OC(F)(F)F
1-butyl-3-methylimidazolium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonate
収率 67.8%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他were combined at room temperature
  2. 2
    その他to give a biphasic mixture with the desired ionic liquid as the bottom phase
  3. 3
    その他The layers were separated
  4. 4
    抽出the aqueous phase was extracted with 2×50 ml portions of methylene chloride
  5. 5
    乾燥The combined organic layers were dried over magnesium sulfate
  6. 6
    濃縮concentrated in vacuo
  7. 7
    その他The colorless oil product was dried at for 4 hr at 5 Pa and 25 degrees C

実験手順

1-Butyl-3-methylimidazolium chloride (Bmim-Cl, 10.0 g) and deionized water (15 ml) were combined at room temperature in a 200 ml flask. At room temperature in a separate 200 ml flask, potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonate (TTES-K, 16.4 g) was dissolved in deionized water (90 ml). These two solutions were combined at room temperature and allowed to stir magnetically for 30 min. under positive nitrogen pressure to give a biphasic mixture with the desired ionic liquid as the bottom phase. The layers were separated, and the aqueous phase was extracted with 2×50 ml portions of methylene chloride. The combined organic layers were dried over magnesium sulfate and concentrated in vacuo. The colorless oil product was dried at for 4 hr at 5 Pa and 25 degrees C. to afford 15.0 g of product.

出典

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