Реакция #1857541

Уравнение реакции

4-chlorophenol

2-chloro-4-fluoroacetophenone

potassium carbonate

→

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

Растворители

DMF

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураto reflux for 48 h
3. 3
   Другоеthe reaction mixture was partitioned between MTBE and water
4. 4
   Экстракцияthe aqueous phase was extracted twice with MTBE
5. 5
   ПромывкаThe combined organic phases were consecutively washed with 10% LiCl solution, dil. NaOH solution and water
6. 6
   Другоеdried
7. 7
   ДругоеThe solvent was evaporated under reduced pressure
8. 8
   Другоеthe crude material was crystallized from diisopropyl ether

Методика

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.

Источник