Reaktion #501083

ord-896a3295d53643268c5f9736e22bda19

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturheated
  2. 2
    Temperaturunder reflux
  3. 3
    Waschenwashed with water, 5% sodium bicarbonate, and brine
  4. 4
    TrocknenThe organic layer was dried over NaSO4
  5. 5
    Filtrationthe solids filtered away
  6. 6
    Sonstigethe solvents removed under vacuum
  7. 7
    SonstigeThe named product was recrystallized from ethanol (m.p. 100° C.-101° C.)

Vorschrift

m-Fluoroaniline (5 mmol, 0.6 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 resuspended in chloroform, then washed with water, 5% sodium bicarbonate, and brine. The organic layer was dried over NaSO4, then the solids filtered away and the solvents removed under vacuum. The named product was recrystallized from ethanol (m.p. 100° C.-101° C.).

Quelle

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