HRID1267112

反应详情

EQUATION

反应方程式

HRID 1267112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

To a stirred solution of 1-(3-cyano-benzyl)-4-(4-nitro-phenyl)-piperazine (52 g) in EtOH (1.2 L) and THF (300 mL) was added portionwise SnC2.2H2O (145.6 g) at room temperature and the mixture was heated at 55° C. for 16 hours. After evaporation of the solvents, the residue was taken in water, basified with NaOH at pH 14 and extracted with CH2Cl2. The organic layer was then washed with water, dried over Na2SO4, and evaporated. The residue was cristallized from disopropyl ether to give the title compound (40.5 g) as pale yellow crystals.

WORKUP

后处理

  1. customAfter evaporation of the solvents
  2. extractionextracted with CH2Cl2
  3. washThe organic layer was then washed with water
  4. dry with materialdried over Na2SO4
  5. customevaporated