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Potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonate → HCID 178448554, compound

HRID 498902
Notes
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Reaction equation

HRID 498902 reaction equation
[Cl-].[CH2:2]([N+:6]1[CH:10]=[CH:9][N:8]([CH3:11])[CH:7]=1)[CH2:3][CH2:4][CH3:5].[F:12][C:13]([F:25])([S:21]([O-:24])(=[O:23])=[O:22])[CH:14]([F:20])[O:15][C:16]([F:19])([F:18])[F:17].[K+]>O>[F:25][C:13]([F:12])([S:21]([O-:24])(=[O:23])=[O:22])[CH:14]([F:20])[O:15][C:16]([F:18])([F:17])[F:19].[CH2:2]([N+:6]1[CH:10]=[CH:9][N:8]([CH3:11])[CH:7]=1)[CH2:3][CH2:4][CH3:5]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 87095932Potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonateHCID 178448538HCID 178448538, compound

Product 1

HCID 178448554HCID 178448554, compoundYield 67.8%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

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.

Workup

  1. customwere combined at room temperature
  2. customto give a biphasic mixture with the desired ionic liquid as the bottom phase
  3. customThe layers were separated
  4. extractionthe aqueous phase was extracted with 2×50 ml portions of methylene chloride
  5. dry with materialThe combined organic layers were dried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe colorless oil product was dried at for 4 hr at 5 Pa and 25 degrees C

Sources & evidence

ORD record
ord-4e2a166ee5ed44bdaa0711513c41caba
Source dataset
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07765823B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes