反应 #1857541

反应方程式

4-chlorophenol

2-chloro-4-fluoroacetophenone

potassium carbonate

→

1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone

溶剂

DMF

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度to reflux for 48 h
3. 3
   其他the reaction mixture was partitioned between MTBE and water
4. 4
   萃取the aqueous phase was extracted twice with MTBE
5. 5
   洗涤The combined organic phases were consecutively washed with 10% LiCl solution, dil. NaOH solution and water
6. 6
   其他dried
7. 7
   其他The solvent was evaporated under reduced pressure
8. 8
   其他the crude material was crystallized from diisopropyl ether

实验过程

A mixture of 4-chlorophenol (186 g), 2-chloro-4-fluoroacetophenone (250 g) and potassium carbonate (238 g) in DMF (960 mL) was heated to reflux for 48 h. After cooling to room temperature, the reaction mixture was partitioned between MTBE and water and the aqueous phase was extracted twice with MTBE. The combined organic phases were consecutively washed with 10% LiCl solution, dil. NaOH solution and water and dried. The solvent was evaporated under reduced pressure and the crude material was crystallized from diisopropyl ether.

来源