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

HRID 648956노트

반응식

HRID 648956 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-527da69bb7b24d09b12664934833b09f
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737495

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