Réaction #169391

ord-31cc3862d3244285a6a75e5c3f5b4c7c

Conditions de réaction

Température
120°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrethen evaporated in vacuo
  2. 2
    AutreThe crude solid was purified by column chromatography on silica gel (80:20 petroleum ether: EtOAc)

Mode opératoire

Ethyl 4-chloroacetoacetate (20.0 g, 122.0 mmol) was added to cyclopropanecarboxamide (3.52 g, 41.5 mmol) in toluene (100 mL) and 1,4-dioxane (100 mL). The mixture was refluxed at 120° C. for 17 hours then evaporated in vacuo. The crude solid was purified by column chromatography on silica gel (80:20 petroleum ether: EtOAc) to afford the title compound as a white solid in 50% yield, 4.00 g.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08846698B2uspto-grants-2014_09