Reaktion #92687

ord-2d92678427e44e14afb990b87d1e5427

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGby stirring at 80° C. for 4 hours
  2. 2
    Sonstigethe solvent was evaporated under reduced pressure
  3. 3
    Extraktionby extracting with ethyl acetate
  4. 4
    Waschenwashing with saturated brine
  5. 5
    TrocknenAfter drying over anhydrous magnesium sulfate
  6. 6
    Filtrationfiltering
  7. 7
    Sonstigethe solvent was evaporated under reduced pressure
  8. 8
    SonstigeThe obtained residue was purified by silica gel column chromatography

Vorschrift

To a suspension of 2.15 g of methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate in 43 ml of ethanol was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, and the solvent was evaporated under reduced pressure, followed by extracting with ethyl acetate and washing with saturated brine. After drying over anhydrous magnesium sulfate and then filtering, the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 1.39 g of methyl 8-[(2-fluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-6-carboxylate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447090B2uspto-grants-2016_09