HRID8605

反应详情

EQUATION

反应方程式

HRID 8605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of 3-methoxyphenol (115 g) in acetone (1000 ml) was added K2CO3 (115 g). The suspension was stirred at 40° C. for 15 min. A solution of dimethylchloromalonate (133 ml) in acetone was added over a period of 45 min. The resulting brown suspension was stirred overnight at 70° C. Finally, the solvent was removed under reduced pressure and the residue was taken up in water (1000 ml) and extracted twice with DCM (500 ml). The combined organic layers were washed with water (500 ml), dried over Na2SO4, and evaporated to give crude dimethyl-(3-methoxyphenoxy)malonate (230 g) as an orange oil. The product was not purified any further.

WORKUP

后处理

  1. stirringThe resulting brown suspension was stirred overnight at 70° C
  2. customFinally, the solvent was removed under reduced pressure
  3. extractionextracted twice with DCM (500 ml)
  4. washThe combined organic layers were washed with water (500 ml)
  5. dry with materialdried over Na2SO4
  6. customevaporated