関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | HCID 178448538 | HCID 178448538 | — |
| 溶媒 | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| 生成物 | HCID 178448547 | HCID 178448547 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07692007B2 |
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| 出典データセット | uspto-grants-2010_04 |
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| ORD ID | ord-2f047d25789c41b9a45450a8db5118ab |
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| 出典メモ | uspto-grants-2010_04 |
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