HRID1267111

反应详情

EQUATION

反应方程式

HRID 1267111 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 1-(4-nitro-phenyl)-piperazine (35.9 g) and potassium carbonate (71.6 g) in acetone (500 mL) was added dropwise 3-cyano-benzyl bromide (34 g) at room temperature and the mixture was heated under reflux. After 4 hours, the salts were removed by filtration, washed with acetone and the filtrate was evaporated to dryness. The residue was taken in CH2Cl2 and the solution was washed with water, dried over Na2SO4, filtered and evaporated. The oily residue was crystallized from AcOEt/diisopropyl ether to give the title compound (52 g) as orange crystals.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. customthe salts were removed by filtration
  4. washwashed with acetone
  5. customthe filtrate was evaporated to dryness
  6. washthe solution was washed with water
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. customevaporated
  10. customThe oily residue was crystallized from AcOEt/diisopropyl ether