Reaktion #305188

ord-971ff2a381c04cd8b519a0c63d671d4c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooling
  2. 2
    workup.STIRRINGby stirring for one hour and 50 minutes
  3. 3
    Extraktionfollowed by extraction with ethyl acetate
  4. 4
    EinengenThe organic layer was concentrated under reduced pressure
  5. 5
    Sonstigethe residue was purified by silica gel column chromatography

Vorschrift

60% sodium hydride (27.8 mg) was added to a solution of 2-methoxyethanol (50.2 μl) in DMF (1 ml) under ice-cooling, followed by stirring for 10 minutes. A solution of methyl 5-chloropyrazine-2-carboxylate (100 mg) in DMF (1 ml) was added to the reaction solution at the same temperature, followed by stirring for one hour and 50 minutes. Acetic acid (50.0 μl) and water were added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to obtain the title compound (19.7 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08198269B2uspto-grants-2012_06