Reaktion #160526

ord-d523f99817fb4c26aa9722aefbfb32cf

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthis mixture was extracted with diethyl ether
  2. 2
    WaschenThis organic layer was washed with brine
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    SonstigeThe solvent was removed under reduced pressure
  6. 6
    WaschenThis residue was washed with ethanol

Vorschrift

A suspension of 1,4-difluoro-2-methyl-5-nitrobenzene (1.00 g), cyanoacetic acid benzyl ester (1.01 g) and potassium carbonate (1.76 g) in N,N-dimethylformamide (20.0 mL) was stirred at 60° C. for 1 day. To this reaction mixture was added 1 mol/L hydrochloric acid (25.4 mL), and this mixture was extracted with diethyl ether. This organic layer was washed with brine, and dried over anhydrous magnesium sulfate, and filtered. The solvent was removed under reduced pressure. This residue was washed with ethanol to give the title compound (1.54 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829040B2uspto-grants-2014_09