HRID55277

反应详情

EQUATION

反应方程式

HRID 55277 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

175 g of manganese dioxide is added to a solution of 29 g of 6-hydroxymethyl-2-iodo-3-methoxypyridine in 600 ml of toluene, and the suspension is heated with stirring and refluxed for three hours on a water separator. The reaction mixture is filtered, the filter residue is washed with dichloromethane, the filtrate is dried on sodium sulfate and concentrated by evaporation. The crude product is chromatographed on silica gel with hexane/0-25% ethyl acetate. 12.9 g of 2-iodo-3-methoxypyridine-6-aldehyde of melting point 118°-121° C. is obtained.

WORKUP

后处理

  1. temperaturethe suspension is heated
  2. filtrationThe reaction mixture is filtered
  3. washthe filter residue is washed with dichloromethane
  4. customthe filtrate is dried on sodium sulfate
  5. concentrationconcentrated by evaporation
  6. customThe crude product is chromatographed on silica gel with hexane/0-25% ethyl acetate