HRID1672222

反应详情

EQUATION

反应方程式

HRID 1672222 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 5-ethynyl-2-methyl-3-nitropyridine (600 mg, 3.70 mmol) in EtOH (10 mL) was added 1-methyl-piperazine (1.64 mL, 14.8 mmol). The reaction mixture was allowed to stir at reflux overnight. The reaction mixture was allowed to cool to rt and palladium hydroxide on carbon (0.060 g) was added to the solution. The reaction mixture was purged with hydrogen and then allowed to stir under an atmosphere of H2 at rt overnight. The reaction mixture was filtered through celite and the filatrate was concentrated. The residue was purified by column chromatography to give 2-methyl-5-[2-(4-methylpiperazin-1-yl)ethyl]pyridin-3-amine (0.664 g, 77%).

WORKUP

后处理

  1. temperatureat reflux overnight
  2. customThe reaction mixture was purged with hydrogen
  3. stirringto stir under an atmosphere of H2 at rt overnight
  4. filtrationThe reaction mixture was filtered through celite
  5. concentrationthe filatrate was concentrated
  6. customThe residue was purified by column chromatography