Potassium Carbonate → HCID 18917288, 화합물

HRID 54747노트

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HRID 54747 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.[Cl:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[CH2:28][C:29]([NH:31][C:32]1[CH:40]=[CH:39][C:35]([C:36](Cl)=[O:37])=[CH:34][CH:33]=1)=[O:30]>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:36](=[O:37])[C:35]2[CH:39]=[CH:40][C:32]([NH:31][C:29](=[O:30])[CH2:28][C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=3[Cl:21])=[CH:33][CH:34]=2)[CH2:12][CH2:11][CH2:10]1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 107977675-Dimethylamino-2,3,4,5-tetrahydro-1H-benzazepineHCID 189173204-[2-(2-Chloro-phenyl)acetylamino]benzoyl chloride

생성물 1

HCID 18917288HCID 18917288, 화합물수율 99.6%

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 mixture was added 66.5 g of 4-[2-(2-chloro-phenyl)acetylamino]benzoyl chloride with ice-cooling and stirring. The mixture was stirred overnight at room temperature. The reaction mixture was mixed with water, followed by extraction with dichloromethane. The dichloromethane layer was dried over magnesium sulfate and then subjected to vacuum distillation to remove the solvent. The residue was purified by silica gel column chromatography and then recrystallized from methanol to obtain 99.3 g of 5-dimethylamino-1-{4-[2-(2-chlorophenyl)acetylamino]benzoyl}-2,3,4,5-tetrahydro-1H-benzoazepine.

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred overnight at room temperature
  3. extractionfollowed by extraction with dichloromethane
  4. dry with materialThe dichloromethane layer was dried over magnesium sulfate
  5. distillationsubjected to vacuum distillation
  6. customto remove the solvent
  7. customThe residue was purified by silica gel column chromatography
  8. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-ef360b12d26b4e64a84d7157d5ed8e1b
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622947

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