Methyl Phosphate → 1,2,3,4-Tetramethylimidazolinium methyl phosphate

HRID 1923418ノート

反応式

HRID 1923418 の反応式
[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]

参加物

4

反応物 2

HCID 12691389Methyl PhosphateHCID 675213621,2,3,4-Tetramethylimidazolinium methyl carbonate

生成物 1

HCID 675210291,2,3,4-Tetramethylimidazolinium methyl phosphate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  1. customA salt exchange reaction

出典と根拠

ORDレコード
ord-6de4985a58d84711aab123fa58e30536
出典データセット
uspto-grants-2012_05
特許番号
US08177994B2

反応ノート

読み込み中…