Potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonate → HCID 178448554、化合物

HRID 498902

反応式

HRID 498902 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].[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]

参加物

4

反応物 2

HCID 87095932Potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonateHCID 178448538HCID 178448538、化合物

生成物 1

HCID 178448554HCID 178448554、化合物収率 67.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

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.

後処理

  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

出典と根拠

ORDレコード
ord-4e2a166ee5ed44bdaa0711513c41caba
出典データセット
uspto-grants-2010_08
特許番号
US07765823B2

関連ノート

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