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

HRID 1978597노트

반응식

HRID 1978597 반응식
[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[S:20](=[O:22])(=[O:21])[CH2:19][CH2:18][C:17]([C:23]([O:25]C)=[O:24])=[CH:16][C:15]=3[CH:27]=2)=[CH:7][CH:6]=1)[CH2:2][CH3:3].Cl>COCCOC>[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[S:20](=[O:21])(=[O:22])[CH2:19][CH2:18][C:17]([C:23]([OH:25])=[O:24])=[CH:16][C:15]=3[CH:27]=2)=[CH:7][CH:6]=1)[CH2:2][CH3:3]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21995889Methyl 7-(4-propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 111646457-(4-Propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid수율 89.8%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

To a solution of methyl 7-(4-propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (400 mg) in 1,2-dimethoxyethane (10 ml) was added 6N hydrochloric acid (5 ml), and the mixture was refluxed for 2 days, cooled to room temperature and concentrated under reduced pressure to give crystals, which were collected by filtration. The crystals were washed with water, 2-propanol and diisopropylether to give colorless crystals of 7-(4-propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (346.1 mg).

후처리

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

출처 및 근거

ORD 기록
ord-8134c075095d415a90628258478eb92c
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235771B1

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