تفاعل #70129

ord-0653ba4abb8e48a19c341f16c1d781ea

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىfor reaction at ambient temperature for 72 hours
  2. 2
    استخلاصthe reaction solution is adjusted to pH 2.2, for extraction into ethyl acetate
  3. 3
    غسيلThe organic layer is rinsed with saturated aqueous sodium chloride
  4. 4
    تجفيفdried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated
  6. 6
    أخرىto obtain the residue
  7. 7
    أخرىThe residue is recrystallized in ethyl acetate
  8. 8
    أخرىtoluene to obtain PHOG of 2.8 g (11.3 mmoL) in crystal

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08535920B2uspto-grants-2013_09