반응 #727844

반응 방정식

1,4-dioxane

1-butyl-3-methylimidazolium chloride

trifluoroacetic acid

CF3C(O)OH

CF3C(O)OH

→

1-butyl-3-methylimidazolium trifluoroacetate

용매

water dioxane

반응 조건

후처리

1. 1
   workup.DISTILLATIONazeotrope are distilled off at atmospheric pressure (85-101° C.)
2. 2
   workup.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. 3
   workup.ADDITION100 ml of 1,4-dioxane are subsequently added
4. 4
   workup.ADDITION105 ml of HCl- and CF3C(O)OH-containing water/dioxane
5. 5
   workup.DISTILLATIONazeotrope are distilled off at atmospheric pressure
6. 6
   건조After 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.

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.

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