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

HRID 54744노트

반응식

HRID 54744 반응식
C(=O)([O-])[O-].[K+].[K+].[CH3:7][N:8]([CH3:20])[CH:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[NH:13][CH2:12][CH2:11][CH2:10]1.[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>[CH3:7][N:8]([CH3:20])[CH:9]1[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=2[N:13]([C:28](=[O:29])[C:27]2[CH:26]=[CH:25][C:24]([N+:21]([O-:23])=[O:22])=[CH:32][CH:31]=2)[CH2:12][CH2:11][CH2:10]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

38.8 g of potassium carbonate was added to a solution of 50 g of 5-dimethylamino-2,3,4,5-tetrahydro-1H-benzoazepine dissolved in 400 ml of acetone and 200 ml of water. To the solution was added 40 g of p-nitrobenzoyl chloride with ice-cooling and stirring. The resulting mixture was stirred overnight at room temperature. The reaction mixture was mixed with an appropriate amount of water. The resulting crystals were collected by filtration and dried to obtain 71 g of 5-dimethylamino-1-(4-nitro-benzoyl)-2,3,4,5-tetrahydro-1H-benzoazepine.

후처리

  1. temperaturecooling
  2. stirringThe resulting mixture was stirred overnight at room temperature
  3. filtrationThe resulting crystals were collected by filtration
  4. customdried

출처 및 근거

ORD 기록
ord-7884228144cf4bfa92fa8f06acf32a4b
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622947

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