P-Toluenesulfonamide → HCID 54500394、化合物

HRID 1164374ノート

反応式

HRID 1164374 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-4d53ecddf9ef41b8990da6920dab04bb
出典データセット
uspto-grants-1983_01
特許番号
US04369186

反応ノート

読み込み中…