Potassium Carbonate → 4-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-Pyrimidine

HRID 411826

Reaktionsgleichung

Reaktionsgleichung von HRID 411826
FC(F)(F)C1C=C(C=CC=1)O[C:7]([O:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=1)=[CH:8][CH:9]=O.[F:27][C:28]([F:39])([F:38])[C:29]1[CH:37]=[CH:36][C:32]([C:33]([NH2:35])=[NH:34])=[CH:31][CH:30]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[F:21][C:18]([F:19])([F:20])[C:14]1[CH:13]=[C:12]([CH:17]=[CH:16][CH:15]=1)[O:11][C:7]1[CH:8]=[CH:9][N:35]=[C:33]([C:32]2[CH:31]=[CH:30][C:29]([C:28]([F:27])([F:38])[F:39])=[CH:37][CH:36]=2)[N:34]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 27773904-(Trifluoromethyl)benzenecarboximidamideHCID 18541697HCID 18541697, Verbindung

Produkt 1

HCID 99299504-(3-Trifluoromethylphenoxy)-2-(4-Trifluoromethylphenyl)-PyrimidineAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 3,3-bis-(3-trifluoromethylphenoxy)-acrolein (10 mmoles), 4-trifluoromethylbenzamidine (10 mmoles), potassium carbonate (10 mmoles) and acetonitril (100 ml), is stirred at 80° C. for four hours. The reaction mixture is cooled down to ambient temperature and filtered through silica. The organic phase is washed with ethyl acetate and concentrated in vacuo. The residue is purified by chromatography on Al2O3 (petrol ethers/ethyl acetate: 2/1) to yield 3.06 g (80%) of the pure product having a melting point of 66° C.

Aufarbeitung

  1. temperatureThe reaction mixture is cooled down to ambient temperature
  2. filtrationfiltered through silica
  3. washThe organic phase is washed with ethyl acetate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified by chromatography on Al2O3 (petrol ethers/ethyl acetate: 2/1)

Quellen und Nachweise

ORD-Eintrag
ord-ab955588beac4678837f619742f8937b
Quelldatensatz
uspto-grants-2003_05
Patentnummer
US06559307B2

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