HRID2097271

反应详情

EQUATION

反应方程式

HRID 2097271 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9.75 g sodium (0.424 mol, 3 eq) were dissolved in 500 ml absolute ethanol (1.5 hours). 58 g of 1-(2,4-Bis-benzyloxy-5-bromo-phenyl)-ethanone (0.141 mol, 1 eq) and 30.98 g diethyl oxalate (0.212 mol, 1.5 eq) were added and the mixture was refluxed for 2 hours. After cooling down, the mixture was poured onto 220 ml of 2N aqueous HCl and the product was extracted into 700 ml dichloromethane. The solvent was removed under reduced pressure and the yellow residue was triturated with 150 ml diethyl ether.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. temperatureAfter cooling down
  3. extractionthe product was extracted into 700 ml dichloromethane
  4. customThe solvent was removed under reduced pressure
  5. customthe yellow residue was triturated with 150 ml diethyl ether