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

HRID 1978595노트

반응식

HRID 1978595 반응식
[CH: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)([CH3:3])[CH3:2].Cl>COCCOC>[CH: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)([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric Acid2회HCID 21995771Methyl 7-(4-isopropoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 219957477-(4-Isopropoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid수율 95.6%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

반응 조건

온도
70 °C

실험 절차

To a solution of methyl 7-(4-isopropoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (250 mg) in 1,2-dimethoxyethane (10 ml) was added 6N hydrochloric acid (3 ml), and the mixture was stirred at 70° C. for 18 hours. To the mixture were added 1,2-dimethoxyethane (10 ml) and 6N hydrochloric acid (5 ml), and the mixture was stirred at 70° C. for 4 days, 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 colorless crystals of 7-(4-isopropoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (230.3 mg).

후처리

  1. stirringthe mixture was stirred at 70° C. for 4 days
  2. temperaturecooled to room temperature
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customto give crystals, which
  8. filtrationwere collected by filtration
  9. washThe crystals were washed with hexane

출처 및 근거

ORD 기록
ord-4b02a919e39540d08fd6e4de8a09e27f
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235771B1

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