HRID1267111
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was heated
- temperatureunder reflux
- customthe salts were removed by filtration
- washwashed with acetone
- customthe filtrate was evaporated to dryness
- washthe solution was washed with water
- dry with materialdried over Na2SO4
- filtrationfiltered
- customevaporated
- customThe oily residue was crystallized from AcOEt/diisopropyl ether