Reaktion #53588

ord-aef1a357148a4a72b8b8de7e3b3f270c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe organic matters were extracted with 50 ml of ethyl acetate twice
  2. 2
    Waschenwashed with 50 ml of water twice
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure

Vorschrift

4.08 g (30.0 mmol) of 3-trifluoromethylpyrazol, 4.75 mmol (30.0 mmol) of 2-chloro-4-fluorobenzaldehyde and 4.14 g (30.0 mmol) of potassium carbonate in 30 ml of N,N-dimethylformamide were stirred at 60° C. for 2 hours. After cooling to room temperature, the reaction mixture was poured into 100 ml of water, and the organic matters were extracted with 50 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. The residue afforded 7.18 g of 2-chloro-4-(3-trifluoromethylpyrazolyl)benzaldehyde (yield 87.2%) as a pale yellow powder, after washed with n-hexane.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06858639B2uspto-grants-2005_02