Hydrochloric Acid → 2,3,4,5-Tetrahydro-1H-3-benzazepine--hydrogen chloride (1/1)

HRID 1668596ノート

反応式

HRID 1668596 の反応式
[CH2:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][C:4](=O)[NH:3][C:2]1=O.CO.[ClH:16]>C(OCC)C>[ClH:16].[CH2:5]1[C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[CH2:1][CH2:2][NH:3][CH2:4]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 7405391H-3-benzazepine-2,4(3H,5H)-dione

生成物 1

HCID 170652302,3,4,5-Tetrahydro-1H-3-benzazepine--hydrogen chloride (1/1)収率 78%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a suspension of 1,5-dihydro-benzo[d]azepine-2,4-dione (9.3 g) in toluene (250 ml) borane-methylsulfide complex (20 ml) was added dropwise under nitrogen atmosphere, then the mixture was heated at reflux for 4 h. MeOH (20 ml) was added dropwise and the mixture refluxed for additional 1 h, then cooled to room temperature. A 10% solution of anidrous HCl in ethyl ether (50 ml) was added and the solid precipitate was filtered off, washed with ethyl ether and desiccated under reduced pressure to afford the title compound as a white solid (7.6 g, 78% yield).

後処理

  1. additionwas added dropwise under nitrogen atmosphere
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 4 h
  4. temperaturethe mixture refluxed for additional 1 h
  5. filtrationthe solid precipitate was filtered off
  6. washwashed with ethyl ether

出典と根拠

ORDレコード
ord-90abf9a9ab5a46259508b58d628e8345
出典データセット
uspto-grants-2011_08
特許番号
US07989444B2

反応ノート

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