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Hydrochloric Acid → Methyl alpha-methylthio-alpha-(m-benzoylphenyl)propionate

HRID 1277781
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HRID 1277781 반응식
CO.[CH3:3][S:4][C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]2([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)OCC[O:18]2)[CH:12]=1)([CH3:10])[C:6]([O:8][CH3:9])=[O:7].Cl>O>[CH3:3][S:4][C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17](=[O:18])[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:12]=1)([CH3:10])[C:6]([O:8][CH3:9])=[O:7]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 12819455Methyl alpha-methylthio-alpha-[m-(2phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionate

생성물 1

HCID 13020172Methyl alpha-methylthio-alpha-(m-benzoylphenyl)propionate수율 95%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

Methanol (10 ml) and 1 ml of water were added to 2.52 g of methyl α-methylthio-α-[m-(2phenyl-1,3-dioxa-2-cyclopentyl)phenyl]propionate, and 0.2 ml of conc. hydrochloric acid was added. The mixture was heated for 20 minutes under reflux. After cooling, 20 ml of water was added, and the mixture was extracted with 50 ml and 10 ml respectively of methylene chloride. The extract was washed twice with 10 ml of water, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was chromatographed on a column of silica gel using methylene chloride as an eluent to afford 2.10 g of methyl α-methylthio-α-(m-benzoylphenyl)-propionate as a colorless oil in a yield of 95%.

후처리

  1. additionwas added
  2. temperatureThe mixture was heated for 20 minutes
  3. temperatureunder reflux
  4. temperatureAfter cooling
  5. extractionthe mixture was extracted with 50 ml and 10 ml respectively of methylene chloride
  6. washThe extract was washed twice with 10 ml of water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. customThe residue was chromatographed on a column of silica gel

출처 및 근거

ORD 기록
ord-202d4065f8fe447a99a69e887ff873fb
출처 데이터셋
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04278802

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