تفاعل #1857541

ord-5dbccbc3503245d396ae24743e35c3ed

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةto reflux for 48 h
  3. 3
    أخرىthe reaction mixture was partitioned between MTBE and water
  4. 4
    استخلاصthe aqueous phase was extracted twice with MTBE
  5. 5
    غسيلThe combined organic phases were consecutively washed with 10% LiCl solution, dil. NaOH solution and water
  6. 6
    أخرىdried
  7. 7
    أخرىThe solvent was evaporated under reduced pressure
  8. 8
    أخرىthe crude material was crystallized from diisopropyl ether

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09247746B2uspto-grants-2016_02