Trifluoroacetic acid → HCID 178448547, 화합물

HRID 640662

반응식

HRID 640662 반응식
[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:18])([F:17])[C:14]([OH:16])=[O:15].O1CCOCC1>O.O1CCOCC1>[F:12][C:13]([F:18])([F:17])[C:14]([O-:16])=[O:15].[CH2:2]([N+:6]1[CH:10]=[CH:9][N:8]([CH3:11])[CH:7]=1)[CH2:3][CH2:4][CH3:5]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acid3회HCID 312751,4-DioxaneHCID 178448538HCID 178448538, 화합물

생성물 1

HCID 178448547HCID 178448547, 화합물

시약·촉매·용매 1

HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

Analogously to Example 1, 23.0 g (0.132 mol) of 1-butyl-3-methylimidazolium chloride are reacted with 28.0 g of approx. 80% aqueous trifluoroacetic acid, CF3C(O)OH (50% excess). 100 ml of 1,4-dioxane are subsequently added, and 112 ml of HCl- and CF3C(O)OH-containing water/dioxane azeotrope are distilled off at atmospheric pressure (85-101° C.). After four further azeotropic distillations with 100 ml of 1,4-dioxane each time, a further 19 g of approx. 80% aqueous trifluoroacetic acid are added to the residue. 100 ml of 1,4-dioxane are subsequently added, and 105 ml of HCl- and CF3C(O)OH-containing water/dioxane azeotrope are distilled off at atmospheric pressure. After three further azeotropic distillations with 100 ml of 1,4-dioxane each time and drying of the distillation residue under reduced pressure at 1.3 Pa and 70° C., 1-butyl-3-methylimidazolium trifluoroacetate is obtained. The yield is approximately quantitative.

후처리

  1. distillationazeotrope are distilled off at atmospheric pressure (85-101° C.)
  2. additionAfter four further azeotropic distillations with 100 ml of 1,4-dioxane each time, a further 19 g of approx. 80% aqueous trifluoroacetic acid are added to the residue
  3. addition100 ml of 1,4-dioxane are subsequently added
  4. addition105 ml of HCl- and CF3C(O)OH-containing water/dioxane
  5. distillationazeotrope are distilled off at atmospheric pressure
  6. dry with materialAfter three further azeotropic distillations with 100 ml of 1,4-dioxane each time and drying of the distillation residue under reduced pressure at 1.3 Pa and 70° C.

출처 및 근거

ORD 기록
ord-2f047d25789c41b9a45450a8db5118ab
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07692007B2

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