Dimethylformamide dimethyl acetal → 1-[3-(Cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]-3-(dimethylamino)prop-2-en-1-one

HRID 1097412노트

반응식

HRID 1097412 반응식
[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.CO[CH:21](OC)[N:22]([CH3:24])[CH3:23]>C1(C)C=CC=CC=1>[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[C:8]([C:16](=[O:18])[CH:17]=[CH:21][N:22]([CH3:24])[CH3:23])[CH:9]=[CH:10][C:11]=2[O:12][CH:13]([F:15])[F:14])[CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 189497631-(3-Cyclopropylmethoxy-4-difluoromethoxyphenyl)ethanone

생성물 1

HCID 668122341-[3-(Cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]-3-(dimethylamino)prop-2-en-1-one수율 92%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

In toluene, dissolved were 1-[3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]ethanone (10 g, 39 mmol) and DMFDMA (N,N-dimethyl formamide dimethyl acetal) (13.9 g, 117 mmol), and the mixture was heated under reflux. The reaction mixture was extracted with EA, and the extract was washed twice with brine, dried over MgSO4, filtered and evaporated under reduced pressure to remove solvent. The mixture was purified via column chromatography (MC/MeOH=10/1) to obtain 1-[3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl]-3-(dimethylamino)prop-2-en-1-one (11 g, 92%).

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. extractionThe reaction mixture was extracted with EA
  4. washthe extract was washed twice with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customto remove solvent
  9. customThe mixture was purified via column chromatography (MC/MeOH=10/1)

출처 및 근거

ORD 기록
ord-7a9ad909660a4a199a35d7832d141e0e
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143262B2

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