HRID384676

反应详情

EQUATION

反应方程式

HRID 384676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-(4,5-dichloropyridin-2-yl)pivalamide (0.400 g, 1.62 mmol), N-methyl-4-aminopiperidine (0.185 g, 1.62 mmol) in NMP (3 mL) was heated at 220° C. under microwave irradiation for 3 h. The crude reaction mixture was purified by ion exchange on SCX-II acidic resin (2 g) eluting with methanol/dichloromethane (1/1), then 2M ammonia-methanol. The basic fractions were combined and the solvent was removed in vacuo. The crude mixture was purified by flash chromatography on silica, eluting with methanol and dichloromethane (1/9), to give the title compound as a colourless solid (0.384 g, 73%).

WORKUP

后处理

  1. customThe crude reaction mixture
  2. customwas purified by ion exchange on SCX-II acidic resin (2 g)
  3. washeluting with methanol/dichloromethane (1/1)
  4. customthe solvent was removed in vacuo
  5. customThe crude mixture was purified by flash chromatography on silica
  6. washeluting with methanol and dichloromethane (1/9)