Réaction #1857541

ord-5dbccbc3503245d396ae24743e35c3ed

Équation de réaction

Oc1ccc(Cl)cc1
4-chlorophenol
CC(=O)c1ccc(F)cc1Cl
2-chloro-4-fluoroacetophenone
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC(=O)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewas heated
  2. 2
    Températureto reflux for 48 h
  3. 3
    Autrethe reaction mixture was partitioned between MTBE and water
  4. 4
    Extractionthe aqueous phase was extracted twice with MTBE
  5. 5
    LavageThe combined organic phases were consecutively washed with 10% LiCl solution, dil. NaOH solution and water
  6. 6
    Autredried
  7. 7
    AutreThe solvent was evaporated under reduced pressure
  8. 8
    Autrethe crude material was crystallized from diisopropyl ether

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09247746B2uspto-grants-2016_02