HRID556798

反应详情

EQUATION

反应方程式

HRID 556798 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of 4,5-dichloropyridin-2-amine (300 mg, 1.84 mmol) and morpholine (480 mg, 5.52 mmol) in DMA (3.6 mL) was heated at 200° C. for 60 minutes by microwave irradiation. The mixture was purified by ion exchange chromatography on SCX-II acidic resin (2 g) eluting with methanol, then 2M ammonia-methanol. The basic fractions were combined and solvent was evaporated. Flash chromatography on silica, eluting with ethyl acetate-hexane (1:1) gave 5-chloro-4-morpholinopyridin-2-amine as a colourless solid (347 mg, 88%).

WORKUP

后处理

  1. customThe mixture was purified by ion exchange chromatography on SCX-II acidic resin (2 g)
  2. washeluting with methanol
  3. customsolvent was evaporated
  4. washFlash chromatography on silica, eluting with ethyl acetate-hexane (1:1)