Reaktion #501082
ord-1f8c75c06df24ecbbe14fe5fb94e9643
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturheated
- 2Temperaturunder reflux
- 3Sonstigeto precipitate the unreacted metanilic acid
- 4EinengenThe remaining material was concentrated under vacuum
- 5Sonstigepurified over silica gel
- 6SonstigeThe 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.).