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

HRID 1978567ノート

反応式

HRID 1978567 の反応式
[CH3:1][O:2][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.Cl>COCCOC>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[S:18](=[O:19])(=[O:20])[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

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21995921HCID 21995921、化合物

生成物 1

HCID 219959627-(4-Methoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid収率 86.3%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

To a solution of methyl 7-(4-methoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (463 mg) in 1,2-dimethoxyethane (30 ml) was added 6N hydrochloric acid (30 ml), and the mixture was refluxed for 18 hours and concentrated under reduced pressure to give crystals, which were collected by filtration. The crystals washed with 2-propanol and hexane to give pale yellow crystals of 7-(4-methoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (384 mg).

後処理

  1. temperaturethe mixture was refluxed for 18 hours
  2. concentrationconcentrated under reduced pressure
  3. customto give crystals, which
  4. filtrationwere collected by filtration
  5. washThe crystals washed with 2-propanol and hexane

出典と根拠

ORDレコード
ord-b2135be6f6844182bdeb0f24a918a68f
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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