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1-Methylimidazole → Bromodecyl(methylimidazolium)hydrobromide

HRID 713171
ノート
印刷プレビュー

反応式

HRID 713171 の反応式
[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]
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

4

反応物 2

HCID 13901-MethylimidazoleHCID 110878771,1-Dibromodecane

生成物 1

HCID 67395248Bromodecyl(methylimidazolium)hydrobromide収率 68%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
55 °C

実験手順

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%.

後処理

  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)

出典と根拠

ORDレコード
ord-4f1ff46efd1f447ebac12335f02bb8cb
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09181364B2

反応ノート

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