4-Nitrobenzoyl chloride → 5-dimethylamino-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine

HRID 5579ノート

反応式

HRID 5579 の反応式
[CH3:1][N:2]([CH3:14])[CH:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][CH2:6][CH2:5][CH2:4]1.C(=O)([O-])[O-].[K+].[K+].[N+:21]([C:24]1[CH:32]=[CH:31][C:27]([C:28](Cl)=[O:29])=[CH:26][CH:25]=1)([O-:23])=[O:22]>CC(C)=O.O>[CH3:1][N:2]([CH3:14])[CH:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[N:7]([C:28](=[O:29])[C:27]2[CH:26]=[CH:25][C:24]([N+:21]([O-:23])=[O:22])=[CH:32][CH:31]=2)[CH2:6][CH2:5][CH2:4]1

参加物

6

反応物 3

HCID 85024-Nitrobenzoyl chlorideHCID 11430Potassium CarbonateHCID 107977675-Dimethylamino-2,3,4,5-tetrahydro-1H-benzazepine

生成物 1

HCID 107358285-dimethylamino-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine収率 97.1%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒2 回

実験手順

To a solution of 5-dimethylamino-2,3,4,5-tetrahydro-1H-benzazepine (50 g) in a mixture of acetone (400 ml) and water (200 ml) is added potassium carbonate (38.8 g), and thereto is added p-nitrobenzoyl chloride (40 g) with stirring under ice-cooling, and the mixture is stirred at room temperature overnight. To the reaction mixture is added an appropriate amount of water, and the precipitated crystals are collected by filtration and dried to give 5-dimethylamino-1-(4-nitrobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (71 g) as pale yellow powder, mp. 139°-142° C.

後処理

  1. temperaturecooling
  2. stirringthe mixture is stirred at room temperature overnight
  3. filtrationthe precipitated crystals are collected by filtration
  4. customdried

出典と根拠

ORDレコード
ord-e5cdc5322a3f49ad962f9c48c672d656
出典データセット
uspto-grants-1993_09
特許番号
US05244898

反応ノート

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