반응 #1857541

ord-5dbccbc3503245d396ae24743e35c3ed

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도to reflux for 48 h
  3. 3
    기타the reaction mixture was partitioned between MTBE and water
  4. 4
    추출the aqueous phase was extracted twice with MTBE
  5. 5
    세척The combined organic phases were consecutively washed with 10% LiCl solution, dil. NaOH solution and water
  6. 6
    기타dried
  7. 7
    기타The solvent was evaporated under reduced pressure
  8. 8
    기타the crude material was crystallized from diisopropyl ether

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09247746B2uspto-grants-2016_02