HRID2299561

反应详情

EQUATION

反应方程式

HRID 2299561 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Benzaldehyde (9.38 g) was added to a solution of N-[2-(9H-carbazol-2-yloxy)]ethylamine (20 g; synthesized according to the process indicated in JP-A-9-249623) in methanol (500 mL). The mixture was then stirred at room temperature for 1 hour. Under an argon atmosphere, platinum oxide (1.00 g; mfd. by Wako Pure Chemical Industries) was added to the mixture, which was then stirred under a hydrogen atmosphere at atmospheric pressure for 3 hours. After replacing the atmosphere in the reaction system with argon, benzaldehyde (1.88 g) was added to the mixture, which was then further stirred under a hydrogen atmosphere at atmospheric pressure for 3 hours. After replacing the atmosphere with argon, the catalyst was filtered off and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethanol and dried under reduced pressure to give the title compound (25.2 g) as a pale yellow crystal.

WORKUP

后处理

  1. customsynthesized
  2. stirringwas then stirred under a hydrogen atmosphere at atmospheric pressure for 3 hours
  3. additionwas added to the mixture, which
  4. stirringwas then further stirred under a hydrogen atmosphere at atmospheric pressure for 3 hours
  5. filtrationthe catalyst was filtered off
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was recrystallized from ethanol
  8. customdried under reduced pressure