HRID2220071

反应详情

EQUATION

反应方程式

HRID 2220071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Chloro-6-methyl-3-nitropyridine (2.5 g, 14.5 mmol) was stirred in 1.0 M solution of methylamine (40 ml, 40 mmol) in methanol at 70° C. for 60 min. After cooling to ambient temperature, and methanol (60 ml) and 10% palladium on activated carbon were added and the resulting mixture was shaken under 40 psi of hydrogen gas at ambient temperature for 30 min. The mixture was filtered through a pad of Celite and concentrated in vacuum. Chromatography on silica gel, eluting with a mixture dichloromethane-methanol-38% aqueous ammonia (9:1:0.1) yielded the title compound (1.65 g, 83%).

WORKUP

后处理

  1. filtrationThe mixture was filtered through a pad of Celite
  2. concentrationconcentrated in vacuum
  3. washChromatography on silica gel, eluting with a mixture dichloromethane-methanol-38% aqueous ammonia (9:1:0.1)