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

HRID 1978579ノート

反応式

HRID 1978579 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[S:18](=[O:20])(=[O:19])[CH2:17][CH2:16][C:15]([C:21]([O:23]C)=[O:22])=[CH:14][C:13]=3[CH:25]=2)=[CH:5][CH:4]=1)[CH3:2].Cl>COCCOC>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[S:18](=[O:20])(=[O:19])[CH2:17][CH2:16][C:15]([C:21]([OH:23])=[O:22])=[CH:14][C:13]=3[CH:25]=2)=[CH:5][CH:4]=1)[CH3:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21995723Methyl 7-(4-ethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

生成物 1

HCID 219957377-(4-Ethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid収率 87%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of methyl 7-(4-ethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (600 mg) in 1,2-dimethoxyethane (20 ml) was added 6N hydrochloric acid (10 ml), and the mixture was refluxed for 24 hours, cooled to room temperature and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give crystals, which were collected by filtration. The crystals were washed with hexane to give pale yellow crystals of 7-(4-ethylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (501.2 mg).

後処理

  1. temperaturethe mixture was refluxed for 24 hours
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give crystals, which
  7. filtrationwere collected by filtration
  8. washThe crystals were washed with hexane

出典と根拠

ORDレコード
ord-3f6c0f96fa5f4c2283b6c483c0a0a2ae
出典データセット
uspto-grants-2001_05
特許番号
US06235771B1

反応ノート

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