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Potassium Chloride → HCID 178448553、化合物

HRID 498903
ノート
印刷プレビュー

反応式

HRID 498903 の反応式
[Cl-].[CH2:2]([N+:6]1[CH:10]=[CH:9][N:8]([CH3:11])[CH:7]=1)[CH2:3][CH2:4][CH3:5].[Cl-].[K+].[F:14][C:15]([F:30])([S:26]([O-:29])(=[O:28])=[O:27])[CH:16]([F:25])[O:17][C:18]([F:24])([F:23])[C:19]([F:22])([F:21])[F:20].[K+]>CC(C)=O>[F:30][C:15]([F:14])([S:26]([O-:29])(=[O:27])=[O:28])[CH:16]([F:25])[O:17][C:18]([F:23])([F:24])[C:19]([F:20])([F:22])[F:21].[CH2:2]([N+:6]1[CH:10]=[CH:9][N:8]([CH3:11])[CH:7]=1)[CH2:3][CH2:4][CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 4873Potassium ChlorideHCID 87096009Potassium;1,1,2-trifluoro-2-(1,1,2,2,2-pentafluoroethoxy)ethanesulfonateHCID 178448538HCID 178448538、化合物

生成物 1

HCID 178448553HCID 178448553、化合物収率 62%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

実験手順

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).

後処理

  1. customto settle leaving a colorless solution above it
  2. filtrationThe reaction mixture was filtered once through a celite/acetone pad
  3. customagain through a fritted glass funnel to remove the KCl
  4. customThe acetone was removed in vacuo first on a rotovap
  5. waiton a high vacuum line (4 Pa, 25 degrees C.) for 2 hr
  6. customResidual KCl was still precipitating out of the solution, so methylene chloride (50 ml)
  7. additionwas added to the crude product, which
  8. washwas then washed with deionized water (2×50 ml)
  9. dry with materialThe solution was dried over magnesium sulfate
  10. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-bb154c89e28c4b1f8428b07c467ceca8
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07765823B2

反応ノート

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