1-Methylimidazole → 1-Methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide

HRID 1171980ノート

反応式

HRID 1171980 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[CH:3]1.[F:7][C:8]([F:28])([F:27])[C:9]([F:26])([F:25])[C:10]([F:24])([F:23])[C:11]([F:22])([F:21])[C:12]([F:20])([F:19])[C:13]([F:18])([F:17])[CH2:14][CH2:15][I:16]>C1(C)C=CC=CC=1>[I-:16].[CH3:1][N+:2]1[CH:6]=[CH:5][N:4]([CH2:15][CH2:14][C:13]([F:17])([F:18])[C:12]([F:19])([F:20])[C:11]([F:21])([F:22])[C:10]([F:23])([F:24])[C:9]([F:26])([F:25])[C:8]([F:28])([F:27])[F:7])[CH:3]=1

参加物

4

反応物 2

HCID 13901-MethylimidazoleHCID 748881,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane

生成物 1

HCID 154950931-Methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide収率 103.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

1-Methylimidazole (4.32 g, 0.52 mol) was partially dissolved in reagent-grade toluene (50 ml) in a large round-bottomed flask and stirred vigorously. 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-8-iodooctane (26 g, 0.053 mol) was added, and the mixture was heated under reflux at 110 degrees C. for 24 hours. The solvent was removed under vacuum giving 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide (30.5 g) as a waxy solid. Potassium 1,1,2,2-tetrafluoroethanesulfonate (TFES-K, 12 g) was added to reagent grade acetone (100 ml) in a separate round-bottomed flask, and this solution was carefully added to the 1-methyl-3-(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)imidazolium iodide which had been dissolved in acetone (50 ml). The reaction mixture was heated under reflux for approximately 16 hours. The reaction mixture was then filtered using a large frit glass funnel to remove the white KI precipitate formed, and the filtrate was placed on a rotary evaporator for 4 hours to remove the acetone. The oily liquid was then filtered a second time to yield the product, as shown by proton NMR.

後処理

  1. temperaturethe mixture was heated
  2. customThe solvent was removed under vacuum

出典と根拠

ORDレコード
ord-f8903e65303b4932a63b462d598ffc40
出典データセット
uspto-grants-2010_11
特許番号
US07829710B2

反応ノート

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