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

HRID 1774185노트

반응식

HRID 1774185 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-5b9610427f88427b81422f03926d2459
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09259470B2

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