反応 #1857541

反応方程式

4-chlorophenol

2-chloro-4-fluoroacetophenone

potassium carbonate

→

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

溶媒

DMF

反応条件

後処理

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

実験手順

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.

出典