HRID746238

反应详情

EQUATION

反应方程式

HRID 746238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of m-nitrobenzaldehyde (1.67 g), 2-(4-benzhydryl-1-piperazinyl)ethyl acetoacetate (4.20 g), benzene (40 ml) and piperidine (0.05 g) was refluxed for 4 hours, during which time the water produced was removed using a Dean-Stark trap. The mixture was washed with water and dried (MgSO4). The solvent was then distilled off and the residue was purified by column chromatography on silica gel (100 g) [eluent: ethyl ether-ethyl acetate (10:1, v/v)] to give 2-(4-benzhydryl-1-piperazinyl)ethyl 2-(3-nitrobenzylidene)acetoacetate as an oil. Yield 4.37 g.

WORKUP

后处理

  1. customproduced
  2. customwas removed
  3. washThe mixture was washed with water
  4. dry with materialdried (MgSO4)
  5. distillationThe solvent was then distilled off
  6. customthe residue was purified by column chromatography on silica gel (100 g) [eluent