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

HRID 1097412ノート

反応式

HRID 1097412 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-7a9ad909660a4a199a35d7832d141e0e
出典データセット
uspto-grants-2012_03
特許番号
US08143262B2

反応ノート

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