4-Fluorobenzoyl chloride → 4-(4-Fluorobenzoyl)-5-methyl-1,3-dihydro-2H-imidazol-2-one

HRID 370549ノート

反応式

HRID 370549 の反応式
[CH3:1][C:2]1[NH:3][C:4](=[O:7])[NH:5][CH:6]=1.[Cl-].[Al+3].[Cl-].[Cl-].[F:12][C:13]1[CH:21]=[CH:20][C:16]([C:17](Cl)=[O:18])=[CH:15][CH:14]=1>[N+](C1C=CC=CC=1)([O-])=O>[F:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([C:6]2[NH:5][C:4](=[O:7])[NH:3][C:2]=2[CH3:1])=[O:18])=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 678794-Fluorobenzoyl chlorideHCID 709351,3-dihydro-4-methyl-2H-imidazol-2-oneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 155675394-(4-Fluorobenzoyl)-5-methyl-1,3-dihydro-2H-imidazol-2-one

試薬・触媒・溶媒 1

HCID 7416Nitrobenzene溶媒

実験手順

To a stirred mixture of 98.1 g (1 mole) of 1,3-dihydro-4-methyl-2H-imidazol-2-one, 266.7 g (2 moles) of anhydrous aluminum chloride and 500 ml of nitrobenzene there is added dropwise over 10 minutes, 158.6 g (1 mole) of p-fluorobenzoyl chloride. The mixture is stirred at 60°-65° C. for 6 hours, then poured onto 2 kg of ice. The precipitate which forms is separated by filtration, washed with diethyl ether and water and recrystallized from dimethylformamide to give 1,3-dihydro-4-(4-fluorobenzoyl)-5-methyl-2H-imidazol-2-one melting at about 289°-292° C.

後処理

  1. additionthere is added dropwise over 10 minutes
  2. customThe precipitate which forms is separated by filtration
  3. washwashed with diethyl ether and water
  4. customrecrystallized from dimethylformamide

出典と根拠

ORDレコード
ord-8fc6f66a1ee54ceeb09961ad8fc596b9
出典データセット
uspto-grants-1985_07
特許番号
US04526981

反応ノート

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