Acetic Acid → 7,8-Dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 648956

反応式

HRID 648956 の反応式
C(O)(=O)C.[CH3:5][O:6][C:7]1[C:18]([O:19][CH3:20])=[CH:17][C:10]2[CH2:11][C:12](=O)[NH:13][CH2:14][CH2:15][C:9]=2[CH:8]=1.[Na]>O1CCOCC1>[CH3:5][O:6][C:7]1[C:18]([O:19][CH3:20])=[CH:17][C:10]2[CH2:11][CH2:12][NH:13][CH2:14][CH2:15][C:9]=2[CH:8]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 5360545SodiumHCID 114017697,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one

生成物 1

HCID 129234297,8-Dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of glacial acetic acid (1.8 g) in dioxan (10 ml) is added dropwise to a suspension of 7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one (1.3 g, 6 mmol) and sodium borohydridel (1 g, 3 mmol) in dioxan (20 ml), refluxed for 3 hours, concentrated by evaporation and decomposed with water. The mixture is extracted twice with methylene chloride, the extract is concentrated by evaporation and the residue is taken up in ether. After filtration the ether is eliminated in vacuo.

後処理

  1. temperaturerefluxed for 3 hours
  2. concentrationconcentrated by evaporation
  3. extractionThe mixture is extracted twice with methylene chloride
  4. concentrationthe extract is concentrated by evaporation
  5. filtrationAfter filtration the ether

出典と根拠

ORDレコード
ord-527da69bb7b24d09b12664934833b09f
出典データセット
uspto-grants-1988_04
特許番号
US04737495

関連ノート

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