1,3-Dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one → 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one

HRID 648955

반응식

HRID 648955 반응식
[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[NH:9][CH:10]=[CH:11][C:5]=2[CH:4]=1>C(O)(=O)C.[Pd]>[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1

참가 물질

4

반응물 1

HCID 14823731,3-Dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one

생성물 1

HCID 114017697,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

A suspension of 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one (21.9 g, 0.1 mol) and 10% palladium/charcoal (1.5 g) in glacial acetic acid (200 ml) is hydrogenated at 50° C. under a hydrogen pressure of 5 bar. After the catalyst has been filtered off the solvent is evaporated in vacuo and the residue is taken up in methylene chloride. After extraction with sodium bicarbonate solution and washing with water, the product is dried over magnesium sulphate, concentrated by evaporation and purified over silica gel with methylene chloride and then with increasing amounts of methanol (up to 10%).

후처리

  1. customis hydrogenated at 50° C. under a hydrogen
  2. filtrationAfter the catalyst has been filtered off the solvent
  3. customis evaporated in vacuo
  4. extractionAfter extraction with sodium bicarbonate solution
  5. washwashing with water
  6. dry with materialthe product is dried over magnesium sulphate
  7. concentrationconcentrated by evaporation
  8. custompurified over silica gel with methylene chloride

출처 및 근거

ORD 기록
ord-04c6be61b72646a7b422c1fdb6bb4583
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737495

연결된 노트

불러오는 중…