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 1681992ノート

反応式

HRID 1681992 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af6294ce9d014e88b761a59cf89d65d0
出典データセット
uspto-grants-1992_12
特許番号
US05175157

反応ノート

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