Imidazole → N,N-Dimethyl-1H-imidazole-1-sulfonamide

HRID 31542ノート

反応式

HRID 31542 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.C(N(CC)CC)C.[CH3:13][N:14]([CH3:19])[S:15](Cl)(=[O:17])=[O:16]>C1(C)C=CC=CC=1>[CH3:13][N:14]([CH3:19])[S:15]([N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1)(=[O:17])=[O:16]

参加物

5

反応物 3

HCID 795ImidazoleHCID 8471TriethylamineHCID 83372Dimethylsulphamoyl chloride

生成物 1

HCID 395751N,N-Dimethyl-1H-imidazole-1-sulfonamide収率 98.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Imidazole (5.00 g, 73.6 mmol) was dissolved in toluene (80 ml), and thereto were added triethylamine (9.52 ml, 68.4 mmol) and dimethylsulfamoyl chloride (6.77 ml, 63.3 mmol), and the mixture was stirred at room temperature for 8 hours. The precipitates were removed by filtration, and the filtrate was concentrated under reduced pressure. The resulting residue was subjected to azeotropic distillation with hexane to give the title compound (10.9 g, 98%).

後処理

  1. customThe precipitates were removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. distillationThe resulting residue was subjected to azeotropic distillation with hexane

出典と根拠

ORDレコード
ord-cdd939ed61584f64924ac03c476e701c
出典データセット
uspto-grants-2008_09
特許番号
US07425642B2

反応ノート

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