HRID432657

反应详情

EQUATION

反应方程式

HRID 432657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Piperidine (1.5 ml) was added to a mixed solvent of acetone (1.1 ml) and ethanol (5 ml). After the resulting mixture was stirred for 5 minutes, 4-chlorobenzaldehyde (700 mg, 5.0 mmol) was added. The thus-obtained mixture was stirred at room temperature for 30 minutes. Acetic acid (two droplets, 0.2 ml) was then added, followed by heating under reflux for 6 hours. The solvent was distilled off and the residue (879 mg) was separated and purified by chromatography on a silica gel column [silica gel 40 g, hexane/diethylether (10/1)], whereby the title compound was obtained as a pale yellow oil (375 mg, 41.7%).

WORKUP

后处理

  1. stirringThe thus-obtained mixture was stirred at room temperature for 30 minutes
  2. temperatureby heating
  3. temperatureunder reflux for 6 hours
  4. distillationThe solvent was distilled off
  5. customthe residue (879 mg) was separated
  6. custompurified by chromatography on a silica gel column [silica gel 40 g, hexane/diethylether (10/1)], whereby the title compound