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

HRID 72068
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HRID 72068 반응식
[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]
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참가 물질

5

반응물 3

HCID 962WaterHCID 31357Tributyl Phosphate2회HCID 675213621,2,3,4-Tetramethylimidazolinium methyl carbonate

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

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온도
100 °C

실험 절차

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.

후처리

  1. customa salt exchange reaction

출처 및 근거

ORD 기록
ord-d90a335ed188489796c079b0d056015e
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08828261B2

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