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N-甲基咪唑 → Bromodecyl(methylimidazolium)hydrobromide

HRID 713171
笔记
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反应方程式

HRID 713171 反应方程式
[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]
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

4

反应物 2

HCID 1390N-甲基咪唑HCID 110878771,1-Dibromodecane

产物 1

HCID 67395248Bromodecyl(methylimidazolium)hydrobromide收率 68%

试剂、催化剂与溶剂 1

HCID 180丙酮溶剂

反应条件

温度
55 °C

实验过程

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%.

后处理

  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)

来源与证据

ORD记录
ord-4f1ff46efd1f447ebac12335f02bb8cb
来源数据集
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
专利号
US09181364B2

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记