3-[(N-Benzyl-piperidin-3-yl)-methyl]-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one → 3-[(piperidin-3-yl)-methyl]-7,8-dimethoxy1,3,4,5-tetrahydro-2H-3-benzazepin-2-one

HRID 1681992노트

반응식

HRID 1681992 반응식
C([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][N:15]2[C:21](=[O:22])[CH2:20][C:19]3[CH:23]=[C:24]([O:29][CH3:30])[C:25]([O:27][CH3:28])=[CH:26][C:18]=3[CH:17]=[CH:16]2)[CH2:9]1)C1C=CC=CC=1.[H][H]>C(O)(=O)C.[Pd]>[NH:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][N:15]2[C:21](=[O:22])[CH2:20][C:19]3[CH:23]=[C:24]([O:29][CH3:30])[C:25]([O:27][CH3:28])=[CH:26][C:18]=3[CH2:17][CH2:16]2)[CH2:9]1

참가 물질

5

반응물 2

HCID 198035973-[(N-Benzyl-piperidin-3-yl)-methyl]-7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-oneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 198038413-[(piperidin-3-yl)-methyl]-7,8-dimethoxy1,3,4,5-tetrahydro-2H-3-benzazepin-2-one

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

14.3 g (0.0352 mol) of 3-[(N-benzyl-piperidin-3-yl)-methyl]7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one are hydrogenated in 120 ml of glacial acetic acid in the presence of 1.5 g of 10% palladium/charcoal for 4 hours at 50° C. under 5 bar of hydrogen. The catalyst is then removed by suction filtering, the glacial acetic acid is distilled off in vacuo and, after the addition of water, the residue is neutralized with potassium carbonate. The greasy precipitate is extracted with methylene chloride, the organic phase is dried over magnesium sulphate and concentrated by evaporation in vacuo. Yield: 9.3 g (83% of theory), Melting point: 152°-156° C.

후처리

  1. customThe catalyst is then removed by suction
  2. filtrationfiltering
  3. distillationthe glacial acetic acid is distilled off in vacuo
  4. additionafter the addition of water
  5. extractionThe greasy precipitate is extracted with methylene chloride
  6. dry with materialthe organic phase is dried over magnesium sulphate
  7. concentrationconcentrated by evaporation in vacuo

출처 및 근거

ORD 기록
ord-af6294ce9d014e88b761a59cf89d65d0
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05175157

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