HRID2196602

反应详情

EQUATION

反应方程式

HRID 2196602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12 g of 5-amino-3-methyl-1,2,4-thiadiazole, 21.1 g of N-hydroxybenzotriazole hydrate and 29.8 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added to a chloroform (500 ml) solution of 21 g of 3,6-dichloro-2-pyridinecarboxylic acid, and stirred at room temperature for 1 hour and then stirred overnight at 50° C. The reaction liquid was diluted with chloroform, then washed with aqueous 0.2 N hydrochloric acid solution, water and saturated saline water. After this was dried with anhydrous magnesium sulfate, the solvent was evaporated away under reduced pressure, and ethyl acetate was added to the resulting residue for crystallization to obtain 22.7 g of the entitled compound as a white solid.

WORKUP

后处理

  1. stirringstirred overnight at 50° C
  2. customThe reaction liquid
  3. washwashed with aqueous 0.2 N hydrochloric acid solution, water and saturated saline water
  4. dry with materialAfter this was dried with anhydrous magnesium sulfate
  5. customthe solvent was evaporated away under reduced pressure, and ethyl acetate
  6. additionwas added to the resulting residue for crystallization