تفاعل #10887

ord-e01217a216ad48d18573a7662bc91efb

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux overnight
  2. 2
    ترشيحThe mixture was filtered
  3. 3
    غسيلthe filter cake was washed with acetonitrile
  4. 4
    أخرىThe solvent was evaporated from the combined filtrates
  5. 5
    أخرىthe residue was partitioned between water and ethyl acetate
  6. 6
    أخرىThe layers were separated
  7. 7
    استخلاصthe aqueous layer was extracted twice with ethyl acetate
  8. 8
    تجفيفThe combined organic layers were dried (Na2SO4)
  9. 9
    ترشيحfiltered
  10. 10
    أخرىevaporated to a yellow solid
  11. 11
    أخرىdried under vacuum

الإجراء التجريبي

A mixture of 1-(4-nitrophenyl)piperazine (12 g, 57.9 mmol) (Acros Organics), powdered potassium carbonate (5.4 g, 39 mmol), iodocyclopentane (7 mL, 60.8 mmol) (Aldrich) and a catalytic amount of 18-crown-6 in acetonitrile (90 mL) was heated at reflux overnight. The mixture was filtered, and the filter cake was washed with acetonitrile. The solvent was evaporated from the combined filtrates and the residue was partitioned between water and ethyl acetate. The layers were separated and the aqueous layer was extracted twice with ethyl acetate. The combined organic layers were dried (Na2SO4), filtered, evaporated to a yellow solid and dried under vacuum to give 1-cyclopentyl-4-(4-nitrophenyl)piperazine) (6.6 g, 41%.)

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07094896B2uspto-grants-2006_08