Reaktion #1857541

Reaktionsgleichung

4-chlorophenol

2-chloro-4-fluoroacetophenone

potassium carbonate

→

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

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturto reflux for 48 h
3. 3
   Sonstigethe reaction mixture was partitioned between MTBE and water
4. 4
   Extraktionthe aqueous phase was extracted twice with MTBE
5. 5
   WaschenThe combined organic phases were consecutively washed with 10% LiCl solution, dil. NaOH solution and water
6. 6
   Sonstigedried
7. 7
   SonstigeThe solvent was evaporated under reduced pressure
8. 8
   Sonstigethe crude material was crystallized from diisopropyl ether

Vorschrift

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.

Quelle