Hydrochloric Acid → 7-[4-(2-Ethoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

HRID 1978688노트

반응식

HRID 1978688 반응식
[CH2:1]([O:3][CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:14]=[CH:15][C:16]3[S:22](=[O:24])(=[O:23])[CH2:21][CH2:20][C:19]([C:25]([O:27]C)=[O:26])=[CH:18][C:17]=3[CH:29]=2)=[CH:9][CH:8]=1)[CH3:2].Cl>COCCOC>[CH2:1]([O:3][CH2:4][CH2:5][O:6][C:7]1[CH:8]=[CH:9][C:10]([C:13]2[CH:14]=[CH:15][C:16]3[S:22](=[O:23])(=[O:24])[CH2:21][CH2:20][C:19]([C:25]([OH:27])=[O:26])=[CH:18][C:17]=3[CH:29]=2)=[CH:11][CH:12]=1)[CH3:2]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21995802Methyl 7-[4-(2-ethoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 219958567-[4-(2-Ethoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid수율 88%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
100 °C

실험 절차

To methyl 7-[4-(2-ethoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (4.35 g) were added 1,2-dimethoxyethane (87 ml) and 6N hydrochloric acid (43.5 ml), and the mixture was refluxed at 100° C. for 16 hours and cooled to room temperature. The mixture was extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated to give 7-[4-(2-ethoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (3.7 g).

후처리

  1. temperaturecooled to room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialdried with magnesium sulfate
  5. customUnder reduced pressure, the solvent was evaporated

출처 및 근거

ORD 기록
ord-37781d8661934a53817e34a7a3a46fc5
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235771B1

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