Reaktion #92678

ord-d2d55b23c17241fd92a6743415c415e4

Lösungsmittel

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter leaving
  2. 2
    Temperaturto be cooled at room temperature
  3. 3
    Sonstigea layer separation operation
  4. 4
    TrocknenThe organic layer was dried over anhydrous sodium sulfate
  5. 5
    Sonstigethe solvent was evaporated under reduced pressure
  6. 6
    SonstigeThe obtained residue was purified by silica gel column chromatography

Vorschrift

To a solution of 1.38 g of 3-(cyclohexylmethoxy)-5-methylpyridin-2-amine in 24 ml of toluene were added 1.21 ml of ethyl 2-chloro-3-oxobutanoate and 1.23 ml of triethylamine, followed by stirring at 110° C. for 3 days. After leaving to be cooled at room temperature, water and diisopropyl ether were added thereto to carry out a layer separation operation. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 1.52 g of ethyl 8-(cyclohexylmethoxy)-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylate.

Quelle

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