HRID10791

反应详情

EQUATION

反应方程式

HRID 10791 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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%.)

WORKUP

后处理

  1. temperatureat reflux overnight
  2. filtrationThe mixture was filtered
  3. washthe filter cake was washed with acetonitrile
  4. customThe solvent was evaporated from the combined filtrates
  5. customthe residue was partitioned between water and ethyl acetate
  6. customThe layers were separated
  7. extractionthe aqueous layer was extracted twice with ethyl acetate
  8. dry with materialThe combined organic layers were dried (Na2SO4)
  9. filtrationfiltered
  10. customevaporated to a yellow solid
  11. customdried under vacuum