HRID2391746

反应详情

EQUATION

反应方程式

HRID 2391746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a suspension of 22.0 g of 2-bromo-5,6-dimethoxy-3-nitropyridine (example E4) in 50 ml DMSO were added 16.0 g sodium azide. The reaction mixture was stirred for 24 h at 50° C. Additional 3.20 g sodium azide were added and after stirring for additional 44 h the reaction was completed. The solvent was removed under vacuum and the resulting residue was extracted with dichloromethane (3×100 ml). The solvent was removed and the residue was purified by flash chromatography (petroleum ether/ethyl acetate) to yield the title compound.

WORKUP

后处理

  1. stirringafter stirring for additional 44 h the reaction
  2. customThe solvent was removed under vacuum
  3. extractionthe resulting residue was extracted with dichloromethane (3×100 ml)
  4. customThe solvent was removed
  5. customthe residue was purified by flash chromatography (petroleum ether/ethyl acetate)