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].[CH3:12][S:13]([OH:16])(=[O:15])=[O:14].O1CCOCC1.Cl>O.O1CCOCC1>[CH3:12][S:13]([O-:16])(=[O:15])=[O:14].[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
6
実験手順
Analogously to Example 1, 26.5 g (0.152 mol) of 1-butyl-3-methylimidazolium chloride are reacted with 21.4 g of approx. 70% aqueous methanesulfonic acid, CH3SO3H. 100 ml of 1,4-dioxane are subsequently added, and 107 ml of HCl-containing water/dioxane azeotrope are distilled off at atmospheric pressure (85-101° C.). After 18 additional 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 80° C., 1-butyl-3-methylimidazolium methylsulfonate is obtained. The yield is approximately quantitative.
後処理
- distillationazeotrope are distilled off at atmospheric pressure (85-101° C.)
- dry with materialAfter 18 additional 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 80° C.
出典と根拠
- ORDレコード
- ord-024cfaa22cdd46ca9089f143746b74fd
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07692007B2
関連ノート
読み込み中…