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Potassium Carbonate → 7-Methanesulfonyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine

HRID 395271
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반응식

HRID 395271 반응식
C([N:4]1[CH2:10][CH2:9][C:8]2[CH:11]=[CH:12][C:13]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:14][C:7]=2[CH2:6][CH2:5]1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>Cl>[CH3:18][S:15]([C:13]1[CH:12]=[CH:11][C:8]2[CH2:9][CH2:10][NH:4][CH2:5][CH2:6][C:7]=2[CH:14]=1)(=[O:17])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 112656343-Acetyl-7-methylsulfonyl-2,3,4,5-tetrahydro-1H-3-benzazepine

생성물 1

HCID 117362667-Methanesulfonyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine수율 32%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of 3-acetyl-7-methylsulphonyl-2,3,4,5-tetrahydro-1H-3-benzazepine (1.75 g, 6.55 mmol) in 5 M hydrochloric acid was heated at reflux for 18 h. The reaction mixture was then cooled to room temperature, basified to pH 12 with potassium carbonate and the solvent evaporated in vacuo. The solid residue was then extracted with ethyl acetate (5×60 ml) and the combined organics dried (Na2SO4). The solvent was then evaporated in vacuo to give the title compound (450 mg, 32%) as a pale yellow oil.

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후처리

  1. temperatureat reflux for 18 h
  2. customthe solvent evaporated in vacuo
  3. extractionThe solid residue was then extracted with ethyl acetate (5×60 ml)
  4. dry with materialthe combined organics dried (Na2SO4)
  5. customThe solvent was then evaporated in vacuo

출처 및 근거

ORD 기록
ord-10f622db23034da5ad3582e8651b7200
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06605607B1

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