HRID27754

反应详情

EQUATION

反应方程式

HRID 27754 的结构方程式

PROCEDURE

实验过程

200 g of 5-cyano-2-hydroxy-6-methyl-3-pyridine-carboxylic acid, ethyl ester (1 mol) are refluxed with stirring in 750 ml of phosphorous oxychloride for 5 hours. The excess of phosphorous oxychloride is removed in vacuo and the residue poured in 1 kg of ice. 2-chloro-5-cyano-6-methyl-3-pyridine-carboxylic acid, ethyl ester crystallizes and is filtered off. Yield 170 g (76%); m.p. 43°-45° C. (petrol ether).

WORKUP

后处理

  1. customThe excess of phosphorous oxychloride is removed in vacuo
  2. additionthe residue poured in 1 kg of ice
  3. custom2-chloro-5-cyano-6-methyl-3-pyridine-carboxylic acid, ethyl ester crystallizes
  4. filtrationis filtered off