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1-Methylimidazole → Bromodecyl(methylimidazolium)hydrobromide

HRID 713171
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HRID 713171 반응식
[Br:1][CH:2]([Br:12])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[CH3:13][N:14]1[CH:18]=[CH:17][N:16]=[CH:15]1>CC(C)=O>[BrH:1].[Br:12][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:15]1[NH:16][CH:17]=[CH:18][N+:14]=1[CH3:13]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 13901-MethylimidazoleHCID 110878771,1-Dibromodecane

생성물 1

HCID 67395248Bromodecyl(methylimidazolium)hydrobromide수율 68%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
55 °C

실험 절차

A dry 250 mL Schlenk flask was equipped with a magnetic stir bar, dropping funnel, and sealed with a rubber septum. Dibromodecane (73.0 g, 0.24 mol) was dissolved in acetone (50 ml) and added to the flask. The mixture was heated to 55° C. in an oil bath, and 1-methylimidazole (4.0 g, 48.7 mmol) was added over 90 minutes via dropping funnel through the top of the flask under nitrogen flow. After addition, the reaction was allowed to stir at 55° C. for 6 hours. The reaction was cooled and solvent was removed in vacuo. The residue was diluted with 150 mL of hexanes and 60 mL of ethyl acetate and placed in a separatory funnel. The bottom layer was removed and purified by column chromatography over silica (dichloromethane/methanol, 9:1 v/v). Yield: 68%.

후처리

  1. customA dry 250 mL Schlenk flask was equipped with a magnetic stir bar
  2. customsealed with a rubber septum
  3. additionadded to the flask
  4. additionAfter addition
  5. temperatureThe reaction was cooled
  6. customsolvent was removed in vacuo
  7. additionThe residue was diluted with 150 mL of hexanes and 60 mL of ethyl acetate
  8. customplaced in a separatory funnel
  9. customThe bottom layer was removed
  10. custompurified by column chromatography over silica (dichloromethane/methanol, 9:1 v/v)

출처 및 근거

ORD 기록
ord-4f1ff46efd1f447ebac12335f02bb8cb
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181364B2

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