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Water → 1,2,3,4-Tetramethylimidazolinium dibutyl phosphate

HRID 72068
ノート
印刷プレビュー

反応式

HRID 72068 の反応式
[P:1]([O:13]CCCC)([O:8][CH2:9][CH2:10][CH2:11][CH3:12])([O:3][CH2:4][CH2:5][CH2:6][CH3:7])=[O:2].COC(=O)[O-].[CH3:23][NH+:24]1[CH2:28][CH:27]([CH3:29])[N:26]([CH3:30])[CH:25]1[CH3:31].O>CO>[CH2:9]([O:8][P:1]([O-:13])([O:3][CH2:4][CH2:5][CH2:6][CH3:7])=[O:2])[CH2:10][CH2:11][CH3:12].[CH3:23][NH+:24]1[CH2:28][CH:27]([CH3:29])[N:26]([CH3:30])[CH:25]1[CH3:31]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 31357Tributyl Phosphate2 回HCID 675213621,2,3,4-Tetramethylimidazolinium methyl carbonate

生成物 1

HCID 675214031,2,3,4-Tetramethylimidazolinium dibutyl phosphate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
100 °C

実験手順

By adding 62 parts of tributyl phosphate to the above-described methanol solution of 46 parts of 1,2,3,4-tetramethylimidazolinium methylcarbonate salt, followed by addition of 5.4 parts of water and stirring at 100° C. for 20 hours, tributyl phosphate was hydrolyzed and a salt exchange reaction was carried out to obtain a methanol solution of 1,2,3,4-tetramethylimidazolinium dibutyl phosphate monoanion. The above-described solution was heated under reduced pressure of 1.0 kPa or less at 50° C. to distill methanol until no distillate of methanol was observed. Thereafter, the temperature was raised from 50° C. to 100° C. and heating was continued for 30 minutes to distill and remove monomethyl carbonate (HOCO2CH3), methanol, and carbon dioxide (slight amounts of methanol and carbon dioxide are formed by thermal decomposition of monomethyl carbonate. Hereinafter, these are abbreviated as by-products). Thus, 1,2,3,4-tetramethylimidazolinium dibutyl phosphate monoanion, electrolyte (C-1), was obtained. The yield was 99 parts (yield based on the weight of 46 parts of 1,2,3,4-tetramethylimidazolinium methyl carbonate salt; hereinafter the same shall apply). The molecular weight of the electrolyte (C-1) was 280.

後処理

  1. customa salt exchange reaction

出典と根拠

ORDレコード
ord-d90a335ed188489796c079b0d056015e
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08828261B2

反応ノート

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