2-Methyl-2-thiopseudourea sulfate → 2-(Methylsulfanyl)-4-[4-(methylsulfanyl)phenyl]-6-(trifluoromethyl)pyrimidine

HRID 1836974

반응식

HRID 1836974 반응식
[F:1][C:2]([F:17])([F:16])[C:3](=O)[CH2:4][C:5]([C:7]1[CH:12]=[CH:11][C:10]([S:13][CH3:14])=[CH:9][CH:8]=1)=O.S(O)(O)(=O)=O.[CH3:23][S:24][C:25](=[NH:27])[NH2:26].C([O-])(=O)C.[Na+]>C(O)(=O)C>[CH3:23][S:24][C:25]1[N:27]=[C:5]([C:7]2[CH:12]=[CH:11][C:10]([S:13][CH3:14])=[CH:9][CH:8]=2)[CH:4]=[C:3]([C:2]([F:17])([F:16])[F:1])[N:26]=1

참가 물질

5

반응물 3

HCID 752702-Methyl-2-thiopseudourea sulfateHCID 517045Sodium AcetateHCID 107301701,3-Butanedione, 4,4,4-trifluoro-1-[4-(methylthio)phenyl]-

생성물 1

HCID 220183142-(Methylsulfanyl)-4-[4-(methylsulfanyl)phenyl]-6-(trifluoromethyl)pyrimidine수율 96.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a mixture of 4,4,4-trifluoro-1-[4-(methylthio)phenyl]butane-1,3-dione (5 g) and 2-methyl-2-thiopseudourea sulfate (5.1 g, 0.98 eq) in acetic acid (100 ml) was added sodium acetate (3 g, 2 eq) and heated under reflux for 8 h. The mixture was concentrated in vacuo and water (100 ml) added to give a solid, which was isolated by filtration to give the title compound as a yellow solid (5.8 g, quantitative).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 8 h
  3. concentrationThe mixture was concentrated in vacuo and water (100 ml)
  4. additionadded
  5. customto give a solid
  6. customwhich was isolated by filtration

출처 및 근거

ORD 기록
ord-ffa684f1df424dab9becdddd400e82bd
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06780869B1

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