Water → HCID 86612643, Verbindung

HRID 1982957Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1982957
Cl[CH2:2][N:3]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[N:4]1.[CH2:12]([CH:15]([C:18]#[N:19])[C:16]#[N:17])[CH:13]=[CH2:14].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:12]([C:15]([CH2:2][N:3]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[N:4]1)([C:18]#[N:19])[C:16]#[N:17])[CH:13]=[CH2:14]

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 10931386HCID 10931386, VerbindungHCID 196193331-(chloromethyl)-3-(trifluoromethyl)-1H-pyrazole

Produkt 1

HCID 86612643HCID 86612643, VerbindungAusbeute 31,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

1.33 g of 1-(chloromethyl)-3-(trifluoromethyl)-1H-pyrazole and 0.76 g of allyl malononitrile were dissolved in 21 ml of N,N-dimethylformamide. 1.99 g of potassium carbonate was added to the solution under ice cooling with stirring, followed by stirring at room temperature for overnight. Water was added to the reaction mixture, and then extracted with MTBE. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was recrystallized from hexane-ethyl acetate to obtain 0.57 g of allyl {[3-(trifluoromethyl)-1H-pyrazole-1-yl]methyl}malononitrile (referred as the compound of the present invention (7), hereinafter) shown by below formula.

Aufarbeitung

  1. stirringby stirring at room temperature for overnight
  2. extractionextracted with MTBE
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was recrystallized from hexane-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-5bad97fbd55b4da6ae70cc1fd9bee25c
Quelldatensatz
uspto-grants-2009_06
Patentnummer
US07541374B2

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