Imidazole → N-[1-(4-chlorophenyl)-1-methylethyl]-3-(imidazol-1-yl)propionamide

HRID 1078394ノート

反応式

HRID 1078394 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([NH:11][C:12](=[O:15])[CH:13]=[CH2:14])([CH3:10])[CH3:9])=[CH:4][CH:3]=1.[NH:16]1[CH:20]=[CH:19][N:18]=[CH:17]1>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([NH:11][C:12](=[O:15])[CH2:13][CH2:14][N:16]2[CH:20]=[CH:19][N:18]=[CH:17]2)([CH3:10])[CH3:9])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 795ImidazoleHCID 18349731N-[1-(4-chlorophenyl)-1-methylethyl]-acrylamide

生成物 1

HCID 19429499N-[1-(4-chlorophenyl)-1-methylethyl]-3-(imidazol-1-yl)propionamide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of N-[1-(4-chlorophenyl)-1-methylethyl]acrylamide (200 g), imidazole (60.9 g), Triton B (20 ml) and 1,4-dioxane (1600 ml) was stirred and boiled under reflux for 20 hours. The solvent was removed under reduced pressure and the residue dissolved in dichloromethane (2000 ml). The mixture was extracted with 2M hydrochloric acid. The combined aqueous extracts were basified with 2M sodium hydroxide solution and extracted with dichloromethane to give N-[1-(4-chlorophenyl)-1-methylethyl]-3-(imidazol-1-yl)propionamide, m.p. 154°-155° C.

後処理

  1. temperatureunder reflux for 20 hours
  2. customThe solvent was removed under reduced pressure
  3. dissolutionthe residue dissolved in dichloromethane (2000 ml)
  4. extractionThe mixture was extracted with 2M hydrochloric acid
  5. extractionextracted with dichloromethane

出典と根拠

ORDレコード
ord-0aabdcbbc38d466f976218d0fad2104f
出典データセット
uspto-grants-1996_08
特許番号
US05547972

反応ノート

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