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

HRID 1978593ノート

反応式

HRID 1978593 の反応式
[CH2:1]([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)[CH2:2][CH3:3].Cl>COCCOC>[CH2:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[S:19](=[O:20])(=[O:21])[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)[CH2:2][CH3:3]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21995893Methyl 7-(4-propylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

生成物 1

HCID 219958817-(4-Propylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid収率 100.1%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of methyl 7-(4-propylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (450 mg) in 1, 2-dimethoxyethane (15 ml) was added 6N hydrochloric acid (7.5 ml), and the mixture was refluxed for 40 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 and recrystallized from THF/diisopropylether to give colorless crystals of 7-(4-propylphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (433.6 mg).

後処理

  1. temperaturethe mixture was refluxed for 40 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. customrecrystallized from THF/diisopropylether

出典と根拠

ORDレコード
ord-bf6dda9260414debb58fd28499a51648
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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