Imidazole → HCID 12151220, Verbindung

HRID 2415039Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2415039
Cl[C:2]1[N:7]=[C:6](Cl)[C:5]([F:9])=[C:4]([C:10]([F:13])([F:12])[F:11])[N:3]=1.[NH:14]1[CH:18]=[CH:17][N:16]=[CH:15]1>C(#N)C>[F:9][C:5]1[C:6]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)=[N:7][C:2]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)=[N:3][C:4]=1[C:10]([F:13])([F:12])[F:11]

Komponenten

4

Edukt 2

HCID 795ImidazoleHCID 133889952,4-Dichloro-5-fluoro-6-(trifluoromethyl)pyrimidine

Produkt 1

HCID 12151220HCID 12151220, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

2,4-Dichloro-5-fluoro-6-trifluoromethylpyrimidine (2.74 g) was dissolved in acetonitrile (30 ml) and imidazole (3.97 g) was added at room temperature with stirring. The mixture was stirred over night and then the solvent was removed under reduced pressure. The residue was added water and extracted with ethyl acetate. The ethyl acetate layer was washed with water and brine, respectively and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was triturated with carbon tetrachloride to give crude, 5-fluoro-2,4-diimidazol-1-yl-6-trifluoromethylpyrimidine. It was recrystallized from isopropanol as colorless crystalline solid, mp 142-150° C. (decomposed).

Aufarbeitung

  1. stirringThe mixture was stirred over night
  2. customthe solvent was removed under reduced pressure
  3. additionThe residue was added water
  4. extractionextracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water and brine
  6. dry with materialrespectively and dried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customThe residue was triturated with carbon tetrachloride

Quellen und Nachweise

ORD-Eintrag
ord-39050fc2a797460ca14da09c6e6d9f03
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06818631B1

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