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

HRID 6694

反応式

HRID 6694 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e51691821d1c445ea36ecbddd8c1bb23
出典データセット
uspto-grants-2006_08
特許番号
US07084148B2

関連ノート

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