反応 #640559

反応方程式

Phenyl pyruvic acid

oxaloacetic acid

potassium hydroxide

hydrochloric acid

→

4-phenylmethyl-4-hydroxy-2-ketoglutaric acid

収率 37.0%

反応条件

後処理

1. 1
   workup.DISSOLUTIONhad been dissolved
2. 2
   その他reacted at room temperature for 72 hours
3. 3
   抽出the reaction mixture was extracted with ethyl acetate
4. 4
   洗浄An organic layer was washed with saturated aqueous NaCl solution
5. 5
   その他dried on magnesium sulfate anhydrate
6. 6
   濃縮concentrated
7. 7
   その他to yield residue
8. 8
   その他The residue was recrystallized from ethyl acetate and toluene

実験手順

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.

出典