تفاعل #640559

ord-7a195b115e354b77a085f722371f1b31

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.DISSOLUTIONhad been dissolved
  2. 2
    أخرىreacted at room temperature for 72 hours
  3. 3
    استخلاصthe reaction mixture was extracted with ethyl acetate
  4. 4
    غسيلAn organic layer was washed with saturated aqueous NaCl solution
  5. 5
    أخرىdried on magnesium sulfate anhydrate
  6. 6
    تركيزconcentrated
  7. 7
    أخرىto yield residue
  8. 8
    أخرىThe residue was recrystallized from ethyl acetate and toluene

الإجراء التجريبي

Phenyl pyruvic acid (5.0 g, 30.5 mmol) and 12.1 g (91.4 mmol) of oxaloacetic acid were added to 25 mL of aqueous solution in which 13.8 g of potassium hydroxide (purity 85%) had been dissolved, and reacted at room temperature for 72 hours. A pH value of the reaction mixture was adjusted to 2.2 using concentrated hydrochloric acid, and the reaction mixture was extracted with ethyl acetate. An organic layer was washed with saturated aqueous NaCl solution, dried on magnesium sulfate anhydrate, and then concentrated to yield residue. The residue was recrystallized from ethyl acetate and toluene to yield 2.8 g (11.3 mmol) of 4-phenylmethyl-4-hydroxy-2-ketoglutaric acid as crystal.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08048647B2uspto-grants-2011_11