反应 #10887

ord-e01217a216ad48d18573a7662bc91efb

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度at reflux overnight
  2. 2
    过滤The mixture was filtered
  3. 3
    洗涤the filter cake was washed with acetonitrile
  4. 4
    其他The solvent was evaporated from the combined filtrates
  5. 5
    其他the residue was partitioned between water and ethyl acetate
  6. 6
    其他The layers were separated
  7. 7
    萃取the aqueous layer was extracted twice with ethyl acetate
  8. 8
    干燥The combined organic layers were dried (Na2SO4)
  9. 9
    过滤filtered
  10. 10
    其他evaporated to a yellow solid
  11. 11
    其他dried under vacuum

实验过程

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%.)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07094896B2uspto-grants-2006_08