Reaktion #501097

ord-cc3e0d10bc464c54b86a885a10859350

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturunder reflux
  3. 3
    SonstigeThe resulting oil was purified over silica, but still contained contaminants
  4. 4
    SonstigeThis material was triturated in hexane
  5. 5
    Sonstigethe solids were separated by filtration
  6. 6
    WaschenThe solids were washed with benzene two times

Vorschrift

3-Aminopyridine (5 mmol, 0.5 g), 2-benzoyl-4-oxo-pentanoic acid ethyl ester (5 mmol, 1.2 g), and tosic acid (0.1 g) were combined in ethanol, then heated under reflux. The resulting oil was purified over silica, but still contained contaminants. This material was triturated in hexane, and the solids were separated by filtration. The solids were washed with benzene two times to yield the named product (m.p. 102° C.-103° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06569890B2uspto-grants-2003_05