Acetic Acid → 1-Ethyl-3-methylimidazolium acetate

HRID 889663노트

반응식

HRID 889663 반응식
S([O-])(O)(=O)=O.[CH3:6][N+:7]1[CH:11]=[CH:10][N:9]([CH2:12][CH3:13])[CH:8]=1.[C:14]([OH:17])(=[O:16])[CH3:15]>O>[C:14]([O-:17])(=[O:16])[CH3:15].[CH3:6][N+:7]1[CH:11]=[CH:10][N:9]([CH2:12][CH3:13])[CH:8]=1

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 162172151-Ethyl-3-methylimidazolium hydrogen sulfate

생성물 1

HCID 116583531-Ethyl-3-methylimidazolium acetate수율 88.3%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

149.8 g (0.72 mol) of 1-methyl-3-ethylimidazolium hydrogensulfate are dissolved in 600 ml of water, and 226.8 g (0.72 mol) of Ba(OH)2 (octahydrate) are subsequently added in portions over a period of 30 minutes. The temperature is increased to 60° C. and the reaction mixture is stirred for 2 hours at this temperature. It is allowed to cool overnight and the precipitated BaSO4 is filtered off using Celite as filter aid. After addition of 43.5 g (0.72 mol) of glacial acetic acid, the water is removed on a rotary evaporator and the oil which remains is extracted with ethyl acetate. To remove residual water, the oil is admixed with n-butanol and the n-butanol is subsequently distilled off under reduced pressure. This gives 108.3 g (0.636 mol) of 1-methyl-3-ethylimidazolium acetate (yield: 88% based on 1-methyl-3-ethylimidazolium hydrogensulfate). The chloride content is 4 ppm.

후처리

  1. temperatureto cool overnight
  2. filtrationthe precipitated BaSO4 is filtered off
  3. filtrationas filter aid
  4. customthe water is removed on a rotary evaporator
  5. extractionthe oil which remains is extracted with ethyl acetate
  6. customTo remove residual water
  7. distillationthe n-butanol is subsequently distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-b748425a75eb4a76b033133c4c3362b7
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08252943B2

반응 노트

불러오는 중…