P-Toluenesulfonamide → HCID 54500394、化合物

HRID 1447965ノート

反応式

HRID 1447965 の反応式
[Cl:1][C:2]1[C:6]([Cl:7])=[N:5][C:4](=[C:8](Cl)Cl)[N:3]=1.[Na].[C:12]1([CH3:22])[CH:17]=[CH:16][C:15]([S:18]([NH2:21])(=[O:20])=[O:19])=[CH:14][CH:13]=1.[O:23]1CCOCC1>O>[CH3:22][C:12]1[CH:13]=[CH:14][C:15]([S:18]([NH:21][C:8]([C:4]2[NH:5][C:6]([Cl:7])=[C:2]([Cl:1])[N:3]=2)=[O:23])(=[O:19])=[O:20])=[CH:16][CH:17]=1

参加物

6

反応物 4

HCID 6269P-ToluenesulfonamideHCID 312751,4-DioxaneHCID 5360545SodiumHCID 124825724,5-Dichloro-2-(dichloromethylidene)-2H-imidazole

生成物 1

HCID 54500394HCID 54500394、化合物収率 42%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 21.8 g (0.1 mol) of 4,5-dichloro-2-dichloromethylene-imidazole in 25 ml of dioxane was added to a suspension of 22 g (0.114 mol) of the sodium salt of p-toluenesulphonamide in 200 ml of water, while stirring. The mixture was then heated briefly to the boil and the product was filtered off while the mixture was still at the boiling point. The precipitate was dried and recrystallized from acetonitrile or toluene. In this way, 14 g (42% of theory) of N-(4-methylphenylsulphonyl)-4,5-dichloroimidazole-2-carboxylic acid amide with a melting point of 238° C. were obtained.

後処理

  1. temperatureThe mixture was then heated briefly to the boil
  2. filtrationthe product was filtered off while the mixture
  3. customThe precipitate was dried
  4. customrecrystallized from acetonitrile or toluene

出典と根拠

ORDレコード
ord-9af039e3fe45485fbc9cb2eceb9ae3b5
出典データセット
uspto-grants-1979_12
特許番号
US04179277

反応ノート

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