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 657553

反応式

HRID 657553 の反応式
[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)C.C(OCC)(=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

参加物

5

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

At ambient temperature, 35 g (159.6 mmol) of 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one are dissolved in a mixture of 525 mL of ethanol and 175 mL of ethyl acetate. There are then added 7 g (20% by weight) of palladium-on-carbon 10% and hydrogenation is carried out at 65° C. and 3.5 bars for 22 hours. The catalyst is filtered off over Celite; rinsing with a mixture of ethanol/ethyl acetate and evaporation to dryness are carried out to yield the desired product.

後処理

  1. customis carried out at 65° C.
  2. filtrationThe catalyst is filtered off over Celite
  3. washrinsing with a mixture of ethanol/ethyl acetate and evaporation to dryness

出典と根拠

ORDレコード
ord-79e09f955b0c4e83b82d3cfe11708c5c
出典データセット
uspto-grants-2011_12
特許番号
US08076325B2

関連ノート

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