Methyl Phosphate → 1,2,3,4-Tetramethylimidazolinium methyl phosphate
Reaction equation
[P:1]([O-:6])([O-:5])([O:3][CH3:4])=[O:2].COC(=O)[O-].[CH3:12][NH+:13]1[CH2:17][CH:16]([CH3:18])[N:15]([CH3:19])[CH:14]1[CH3:20]>CO>[CH3:4][O:3][P:1]([O-:6])([O-:5])=[O:2].[CH3:12][NH+:13]1[CH2:17][CH:16]([CH3:18])[N:15]([CH3:19])[CH:14]1[CH3:20].[CH3:12][NH+:13]1[CH2:17][CH:16]([CH3:18])[N:15]([CH3:19])[CH:14]1[CH3:20]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A salt exchange reaction was performed by adding methyl phosphate mixed ester (about 1 to 3 wt % of phosphoric acid, about 44 to 49 wt % of monomethyl phosphate, about 44 to 49 wt % of dimethyl phosphate and about 3 to 5 wt % of trimethyl phosphate) (AP-1; produced by Daihachi Chemical Industries Co., Ltd.) (0.1 mol) to a methanol solution of 1,2,3,4-tetramethylimidazolinium methyl carbonate salt (0.1 mol), and thereby obtaining a methanol solution of 1,2,3,4-tetramethylimidazolinium methyl phosphate mixed ester anion. The resulting solution was heated at a pressure reduction degree of 1.0 kPa or less at 50° C., so that methanol was evaporated until methanol was no longer distilled off. Then, the temperature was increased from 50° C. to 100° C. and subsequently heating was continued for 30 minutes to distill monomethyl carbonate (HOCO2CH3) off together with methanol and carbon dioxide, which are formed slightly through thermal decomposition of monomethyl carbonate and hereinafter abbreviated as by-products. An electrolyte (c1) {1,2,3,4-tetramethylimidazolinium methyl phosphate mixed ester anion} was thereby obtained. The yield of the product was 98 wt %, which was a yield on the basis of the weight of 1,2,3,4-tetramethylimidazolinium methyl carbonate salt (0.1 mol); ditto in the following.
Workup
- customA salt exchange reaction
Sources & evidence
- ORD record
- ord-6de4985a58d84711aab123fa58e30536
- Source dataset
- uspto-grants-2012_05
- Patent number
- US08177994B2
Reaction notes
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