Dimethylformamide dimethyl acetal → (E)-3-(dimethylamino)-1-(2-(methylthio)pyrimidin-4-yl)prop-2-en-1-one

HRID 2365830노트

반응식

HRID 2365830 반응식
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[CH3:9][S:10][C:11]1[N:16]=[C:15]([C:17](=[O:19])[CH3:18])[CH:14]=[CH:13][N:12]=1>>[CH3:6][N:4]([CH3:5])/[CH:3]=[CH:18]/[C:17]([C:15]1[CH:14]=[CH:13][N:12]=[C:11]([S:10][CH3:9])[N:16]=1)=[O:19]

참가 물질

3

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 116583481-[2-(Methylsulfanyl)pyrimidin-4-yl]ethan-1-one

생성물 1

HCID 21948442(E)-3-(dimethylamino)-1-(2-(methylthio)pyrimidin-4-yl)prop-2-en-1-one수율 69.4%

실험 절차

1,1-Dimethoxy-N,N-dimethylmethanamine (9.87 mL, 74.3 mmol) was added to 1-(2-(methylthio)pyrimidin-4-yl)ethanone (0.50 g, 2.97 mmol). The mixture was heated at reflux overnight. The reaction mixture was concentrated to half volume and treated with Et2O. The resulting solid was collected by vacuum filtration to yield the desired (E)-3-(dimethylamino)-1-(2-(methylthio)pyrimidin-4-yl)prop-2-en-1-one (0.46 g, 2.06 mmol, 69.3% yield).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux overnight
  3. concentrationThe reaction mixture was concentrated to half volume
  4. additiontreated with Et2O
  5. filtrationThe resulting solid was collected by vacuum filtration

출처 및 근거

ORD 기록
ord-3a98a2ded51e4eddbc1e67cb3afbbace
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697715B2

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