1-Methylimidazole → 1-Ethyl-3-methylimidazolium trifluoromethanesulfonate

HRID 1296812

반응식

HRID 1296812 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[CH:3]1.[O:7]([CH2:15][CH3:16])[S:8]([C:11]([F:14])([F:13])[F:12])(=[O:10])=[O:9]>CCCCCC>[F:12][C:11]([F:14])([F:13])[S:8]([O-:10])(=[O:9])=[O:7].[CH3:1][N+:2]1[CH:6]=[CH:5][N:4]([CH2:15][CH3:16])[CH:3]=1

참가 물질

4

반응물 2

HCID 13901-MethylimidazoleHCID 67924Ethyl trifluoromethanesulphonate

생성물 1

HCID 27588741-Ethyl-3-methylimidazolium trifluoromethanesulfonate수율 99.1%

시약·촉매·용매 1

HCID 8058Hexane용매

반응 조건

온도
72.5 °C

실험 절차

6.31 g (0.0768 mol) of 1-methylimidazole in 50 ml of dry hexane are introduced into a round-bottomed flask fitted with a reflux condenser. 13.75 g (0.0772 mol) of ethyl triflate are added over the course of 20 minutes with constant stirring and cooling with the aid of an ice bath. After a further 10 minutes, the ice bath is then replaced by an oil bath, and the reaction mixture is refluxed for one hour (oil-bath temperature 70-75° C.). After the hexane has been removed by distillation, the reaction mixture which remains is held at 80-90° C. in a 30-100 Pa vacuum for 5 hours, giving 19.80 g (yield: 99.1%) of 1-methyl-3-ethylimidazolium trifluoromethanesulfonate as a transparent, colourless liquid.

후처리

  1. customfitted with a reflux condenser
  2. temperaturecooling with the aid of an ice bath
  3. customAfter the hexane has been removed by distillation
  4. waitthe reaction mixture which remains is held at 80-90° C. in a 30-100 Pa vacuum for 5 hours

출처 및 근거

ORD 기록
ord-befd09c930ef40a8842be91fc4614881
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07247740B2

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