HRID2040931

反应详情

EQUATION

反应方程式

HRID 2040931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

27.8 g (79.9 mmol) of methyl N-{2-[2-(4-chlorophenoxy)phenyl]-1-oxoethyl}-N-methylglycinate (compound IIIb) was dissolved in 150 mL of toluene. 11.5 g of sodium tert-butoxyde were added, and the resulting mixture was stirred overnight at room temperature. 350 mL of water were added, and the resulting mixture was extracted three times with 150 mL of ethyl acetate. The combined organic phases were washed with 200 mL of water. The aqueous phases were combined and pH was adjusted to 1 with HCl 2 M. The solvent was removed by filtration, and the solid was recrystallized twice with methanol, to obtain 5.4 g of 3-[2-(4-chlorophenoxy)phenyl]-1-methylpyrrolidine-2,4-dione (compound IVb) as a solid. Yield: 21.4%.

WORKUP

后处理

  1. extractionthe resulting mixture was extracted three times with 150 mL of ethyl acetate
  2. washThe combined organic phases were washed with 200 mL of water
  3. customThe solvent was removed by filtration
  4. customthe solid was recrystallized twice with methanol