Reaktion #501082

ord-1f8c75c06df24ecbbe14fe5fb94e9643

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturunder reflux
  3. 3
    Sonstigeto precipitate the unreacted metanilic acid
  4. 4
    EinengenThe remaining material was concentrated under vacuum
  5. 5
    Sonstigepurified over silica gel
  6. 6
    SonstigeThe named product was collected as brown crystals (m.p. 91° C.-92.5° C.)

Vorschrift

Metanilic acid (5 mmol, 0.2 g), 2-benzoyl-4-oxo-pentanoic acid ethyl ester (5 mmol, 1.2 g), sodium hydroxide (5 mmol, 0.2 g), and tosic acid (0.1 g) were combined in ethanol, then heated under reflux. The resulting oil was treated with HCl (hydrochloric acid) at 0° C. to 50° C. to precipitate the unreacted metanilic acid. The remaining material was concentrated under vacuum and purified over silica gel. The named product was collected as brown crystals (m.p. 91° C.-92.5° C.).

Quelle

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