HRID2072325

反应详情

EQUATION

反应方程式

HRID 2072325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

13.8 ml. of triethylamine are added, at 10° C., to a solution of 29.25 g. of 2-[4-(4-chlorophenoxy)-phenoxy]-propionic acid in 200 ml. of THF. The mixture is cooled to -10° C., a solution of 9.8 ml. of chloroformic acid ethyl ester in 60 ml, of THF is added dropwise and the mixture is stirred for 1 hour at -10° C. The solution contains 1-[4-(4-chlorophenoxy)-phenoxy]-4,6-dioxa-octane-3,5-dione, which is not isolated. 7.4 g. of NaBH4 are then introduced in portions. The mixture is stirred for 30 minutes at -10° C. and for 30 minutes at 0° C., poured into water and extracted with chloroform. After evaporation of the extract, the residue is boiled for 1 hour with 200 ml. of 6% ethanolic potassium hydroxide solution, the mixture is evaporated and worked up with water and ether to give 2-[4-(4-chlorophenoxy)-phenoxy]-propanol.

WORKUP

后处理

  1. customis not isolated
  2. stirringThe mixture is stirred for 30 minutes at -10° C. and for 30 minutes at 0° C.
  3. extractionextracted with chloroform
  4. customAfter evaporation of the extract
  5. waitthe residue is boiled for 1 hour with 200 ml
  6. customof 6% ethanolic potassium hydroxide solution, the mixture is evaporated