Reaktion #49796

ord-46647fc881914ca98a879d80d107cc7d

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    ExtraktionThe organic extract
  4. 4
    Waschenis washed with brine
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    Einengenconcentrated in vacuo
  7. 7
    Sonstigeto obtain an orange oil

Vorschrift

A mixture of methyl [o-(5-fluoro-2-nitrophenoxy)phenoxy]acetate (1.1 g, 3.4 mmol), 1-methyl-5-(trifluoromethyl)pyrazol-3-ol (0.63 g, 3.8 mmol) and potassium carbonate (0.53 g, 3.8 mmol) in N,N-dimethylformamide is stirred at 100° C. for 18 hours, cooled to room temperature, poured into water and extracted with ethyl acetate. The organic extract is washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain an orange oil. Column chromatography of the oil using silica gel and a 30% ethyl acetate in hexanes solution gives the title product as a yellow oil (0.5 g) which is identified by 1HNMR and 13CNMR spectral analyses.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424280uspto-grants-1995_06