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

HRID 1978605노트

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HRID 1978605 반응식
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([C:8]2[CH:9]=[CH:10][C:11]3[S:17](=[O:19])(=[O:18])[CH2:16][CH2:15][C:14]([C:20]([O:22]C)=[O:21])=[CH:13][C:12]=3[CH:24]=2)[S:6][CH:7]=1>COCCOC>[CH3:2][C:3]1[CH:4]=[C:5]([C:8]2[CH:9]=[CH:10][C:11]3[S:17](=[O:18])(=[O:19])[CH2:16][CH2:15][C:14]([C:20]([OH:22])=[O:21])=[CH:13][C:12]=3[CH:24]=2)[S:6][CH:7]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 21995692Methyl 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 219958967-(4-Methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

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온도
100 °C

실험 절차

In 1,2-dimethoxyethane (15.3 ml) was dissolved methyl 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate. (510 mg), and to the solution was added 6N hydrochloric acid (10.2 ml). The mixture was stirred at 100° C. for 15 hours and cooled to room temperature. Under reduced pressure, the solvent was evaporated. To the residue,were added ethyl acetate and potassium carbonate solution, and the mixture was extracted with water. To the solution was added 6N hydrochloric acid, and the solution was made pH 4-5, extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated to give 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (459 mg).

후처리

  1. temperaturecooled to room temperature
  2. customUnder reduced pressure, the solvent was evaporated
  3. additionTo the residue,were added ethyl acetate and potassium carbonate solution
  4. extractionthe mixture was extracted with water
  5. additionTo the solution was added 6N hydrochloric acid
  6. extractionextracted with ethyl acetate
  7. washwashed with saturated brine
  8. dry with materialdried with magnesium sulfate
  9. customUnder reduced pressure, the solvent was evaporated

출처 및 근거

ORD 기록
ord-b8f8600acfff448da21d8681cfb3191d
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235771B1

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