Methanol → Methyl 3,5-dimethoxyphenylacetate

HRID 11768

반응식

HRID 11768 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][C:12]([OH:14])=[O:13])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.S(=O)(=O)(O)O.[CH3:20]O>>[CH3:20][O:13][C:12](=[O:14])[CH2:11][C:5]1[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=[C:3]([O:2][CH3:1])[CH:4]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 138316(3,5-Dimethoxyphenyl)acetic acid

생성물 1

HCID 592191Methyl 3,5-dimethoxyphenylacetate

실험 절차

To a solution of 3,5-dimethoxyphenylacetic acid (1.99 g, 10.0 mmol) (Transworld) in methanol (20 mL) was added concentrated sulfuric acid (1.0 mL) and the reaction mixture was heated at reflux for 24 hours. The reaction mixture was concentrated in vacuo. The residue was then diluted with ethyl acetate (100 mL) and successively washed with water (50 mL) and brine (50 mL), dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo to give the crude 3,5-dimethoxyphenylacetic acid methyl ester as a black oil which was used in the next step without further purification. (Yield 2.05 g, 97.6%).

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 24 hours
  3. concentrationThe reaction mixture was concentrated in vacuo
  4. additionThe residue was then diluted with ethyl acetate (100 mL)
  5. washsuccessively washed with water (50 mL) and brine (50 mL)
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-22aae1a312904b26991097295d0ce830
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098332B2

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