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Hydrochloric Acid → 7-(4-Ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

HRID 1978569
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HRID 1978569 반응식
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[S:19](=[O:21])(=[O:20])[CH2:18][CH2:17][C:16]([C:22]([O:24]C)=[O:23])=[CH:15][C:14]=3[CH:26]=2)=[CH:6][CH:5]=1)[CH3:2].Cl>COCCOC>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[S:19](=[O:21])(=[O:20])[CH2:18][CH2:17][C:16]([C:22]([OH:24])=[O:23])=[CH:15][C:14]=3[CH:26]=2)=[CH:6][CH:5]=1)[CH3:2]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21995858Methyl 7-(4-ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 219958687-(4-Ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid수율 87.9%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

To a solution of methyl 7-(4-ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (600 mg) in 1,2-dimethoxyethane (40 ml) was added 6N hydrochloric acid (30 ml), and the mixture was refluxed for 7 hours and concentrated under reduced pressure. To the residue was added 2-propanol, and precipitated crystals were collected by filtration. The crystals were dissolved in THF, and the solution was concentrated to give crystals, which were collected by filtration to give pale yellow crystals of 7-(4-ethoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (507.5 mg).

후처리

  1. temperaturethe mixture was refluxed for 7 hours
  2. concentrationconcentrated under reduced pressure
  3. additionTo the residue was added 2-propanol
  4. customprecipitated crystals
  5. filtrationwere collected by filtration
  6. dissolutionThe crystals were dissolved in THF
  7. concentrationthe solution was concentrated
  8. customto give crystals, which
  9. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-241a312668ef40be87a4596ed31e3482
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06235771B1

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