反应 #640559

反应方程式

Phenyl pyruvic acid

oxaloacetic acid

potassium hydroxide

hydrochloric acid

→

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

收率 37.0%

反应条件

后处理

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

实验过程

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.

来源