Potassium Carbonate → HCID 18917288、化合物

HRID 54747ノート

反応式

HRID 54747 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 18917288HCID 18917288、化合物収率 99.6%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ef360b12d26b4e64a84d7157d5ed8e1b
出典データセット
uspto-grants-1997_04
特許番号
US05622947

反応ノート

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