Methyl triflate → 3-(Imidazole-1-sulfonyl)-1-methyl-3H-imidazol-1-ium triflate

HRID 1969511ノート

反応式

HRID 1969511 の反応式
[S:1]([N:9]1[CH:13]=[CH:12][N:11]=[CH:10]1)([N:4]1[CH:8]=[CH:7][N:6]=[CH:5]1)(=[O:3])=[O:2].[F:14][C:15]([F:22])([F:21])[S:16]([O:19]C)(=[O:18])=[O:17]>C(Cl)Cl>[F:14][C:15]([F:22])([F:21])[S:16]([O-:19])(=[O:18])=[O:17].[N:4]1([S:1]([N:9]2[CH:13]=[CH:12][N+:11]([CH3:15])=[CH:10]2)(=[O:2])=[O:3])[CH:8]=[CH:7][N:6]=[CH:5]1

参加物

4

反応物 2

HCID 9526Methyl triflateHCID 816091,1'-sulphonylbis-1H-imidazole

生成物 1

HCID 117281493-(Imidazole-1-sulfonyl)-1-methyl-3H-imidazol-1-ium triflate収率 198%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 1,1′-sulfonyldiimidazole (3.50 g, 17.7 mmol) in DCM (75 mL) at about 0° C. was added methyl trifluoromethanesulfonate (1.94 mL, 17.7 mmol). The reaction mixture was stirred at about 0° C. for about 1 h, then warmed to ambient temperature and stirred for about 5 h. The solid was collected by vacuum filtration and washed with DCM (10 mL) to give 1-(1H-imidazol-1-ylsulfonyl)-3-methyl-1H-imidazol-3-ium trifluoromethanesulfonate (6.35 g, 98%) as a white solid: LC/MS (Table 1, Method a) Rt=0.082 min; MS m/z 213 (M+H)+.

後処理

  1. temperaturewarmed to ambient temperature
  2. stirringstirred for about 5 h
  3. filtrationThe solid was collected by vacuum filtration
  4. washwashed with DCM (10 mL)

出典と根拠

ORDレコード
ord-e0677b92aa2e4c968b55397773d64953
出典データセット
uspto-grants-2013_04
特許番号
US08426411B2

反応ノート

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