1-[3-(Cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]ethanol → 1-(3-Cyclopropylmethoxy-4-difluoromethoxyphenyl)ethanone

HRID 1097411노트

반응식

HRID 1097411 반응식
[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([CH:16]([OH:18])[CH3:17])[CH:9]=[CH:10][C:11]=2[O:12][CH:13]([F:15])[F:14])[CH2:3][CH2:2]1.[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1>>[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([C:16](=[O:18])[CH3:17])[CH:9]=[CH:10][C:11]=2[O:12][CH:13]([F:15])[F:14])[CH2:3][CH2:2]1

참가 물질

3

반응물 2

HCID 592936281-[3-(Cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]ethanolHCID 178418287HCID 178418287, 화합물

생성물 1

HCID 189497631-(3-Cyclopropylmethoxy-4-difluoromethoxyphenyl)ethanone수율 91%

실험 절차

In dry MC, dissolved was 1-[3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]ethanol (24 g, 93 mmol), and PCC (pyridinium chlorochromate) (30 g, 139 mmol) was added thereto. The resultant mixture was heated under reflux. The reaction mixture was filtered through Celite, and the filtrate was extracted with EA, washed twice with brine, dried over MgSO4 and filtered. After removing the solvent by evaporation under reduced pressure, the mixture was purified via column chromatography (n-hexane/MC=7/1) to obtain 1-[3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]ethanone (19 g, 91%).

후처리

  1. dissolutionIn dry MC, dissolved
  2. additionwas added
  3. temperatureunder reflux
  4. filtrationThe reaction mixture was filtered through Celite
  5. extractionthe filtrate was extracted with EA
  6. washwashed twice with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customAfter removing the solvent
  10. customby evaporation under reduced pressure
  11. customthe mixture was purified via column chromatography (n-hexane/MC=7/1)

출처 및 근거

ORD 기록
ord-ca21e6e32eff4ff29b999ea7726d3f5e
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143262B2

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