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

HRID 5579노트

반응식

HRID 5579 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e5cdc5322a3f49ad962f9c48c672d656
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244898

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