Réaction #70129

ord-0653ba4abb8e48a19c341f16c1d781ea

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Autrefor reaction at ambient temperature for 72 hours
  2. 2
    Extractionthe reaction solution is adjusted to pH 2.2, for extraction into ethyl acetate
  3. 3
    LavageThe organic layer is rinsed with saturated aqueous sodium chloride
  4. 4
    Séchagedried over anhydrous magnesium sulfate
  5. 5
    Concentrationconcentrated
  6. 6
    Autreto obtain the residue
  7. 7
    AutreThe residue is recrystallized in ethyl acetate
  8. 8
    Autretoluene to obtain PHOG of 2.8 g (11.3 mmoL) in crystal

Mode opératoire

5.0 g (30.5 mmol) of phenylpyruvic acid and 12.1 g (91.4 mmol) of oxaloacetic acid are added to 25 ml of water preliminarily dissolving 13.8 g of potassium hydroxide (purity of 85%) therein, for reaction at ambient temperature for 72 hours. Using the conc. hydrochloric acid, the reaction solution is adjusted to pH 2.2, for extraction into ethyl acetate. The organic layer is rinsed with saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated to obtain the residue. The residue is recrystallized in ethyl acetate and toluene to obtain PHOG of 2.8 g (11.3 mmoL) in crystal.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08535920B2uspto-grants-2013_09