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

HRID 1668596노트

반응식

HRID 1668596 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-90abf9a9ab5a46259508b58d628e8345
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989444B2

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