HRID399623

反应详情

EQUATION

反应方程式

HRID 399623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

23 g of 2-chloro-3-cyano-4,6-dimethylpyridine are dissolved in 185 ml of concentrated hydrochloric acid and 240 ml of water. 25.4 g of tin metal are added and the mixture is brought to 100° C. The reaction is monitored by thin layer chromatography (TLC). When the reaction is complete, the mixture is allowed to return to room temperature and filtered and the filtrate is neutralized using sodium hydroxide solution. The mixture is extracted with methylene chloride and the combined organic phases are washed with saturated aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulphate. The solution is concentrated to give 5-cyano-2,4-dimethyl-pyridine in the form of a yellow precipitate.

WORKUP

后处理

  1. customis brought to 100° C
  2. customto return to room temperature
  3. filtrationfiltered
  4. extractionThe mixture is extracted with methylene chloride
  5. washthe combined organic phases are washed with saturated aqueous sodium bicarbonate solution
  6. dry with materialdried over anhydrous magnesium sulphate
  7. concentrationThe solution is concentrated