Reaktion #155741

ord-b343e2f0437e49488452de340c3fca77

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction was refluxed 2 h
  2. 2
    workup.STIRRINGstirred over night at RT
  3. 3
    Extraktionextracted with diethylether
  4. 4
    EinengenThe organic layer was concentrated
  5. 5
    Sonstigethe residue was purified by chromatography on silica gel

Vorschrift

0.88 g 60% sodiumhydrid was added 1-cyclohexyl-ethanone in 60 mL THF and stirred for 30 min. Then, 3.25 g 4-fluoro-benzoic acid methyl ester and 200 mg 18-Krone-6 was added to the reaction. The reaction was refluxed 2 h and stirred over night at RT. The reaction was added to 100 mL 1N HCl and extracted with diethylether. The organic layer was concentrated and the residue was purified by chromatography on silica gel and 3 g of the desired compound was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822464B2uspto-grants-2014_09