HRID476903

反应详情

EQUATION

反应方程式

HRID 476903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

16 ml of carbon disulfide are added dropwise at room temperature, with stirring, to a suspension of 40 g of 3-trifluoromethyl-2-hydrazinopyridine, prepared in Example 12, in 75 ml of pyridine. When the additioon is complete, stirring is continued for 15 minutes at room temperature and the reaction mixture is then heated under reflux for 5 hours. After cooling, the medium is concentrated in vacuo and water is then added. The solid residue obtained is filtered off, washed with water and dried to give 40 g of 3-mercapto-8-trifluoromethyl-1,2,4-triazolo(4,3-a)pyridine in the form of crystals melting at 236° C.

WORKUP

后处理

  1. temperaturethe reaction mixture is then heated
  2. temperatureunder reflux for 5 hours
  3. temperatureAfter cooling
  4. concentrationthe medium is concentrated in vacuo and water
  5. additionis then added
  6. customThe solid residue obtained
  7. filtrationis filtered off
  8. washwashed with water
  9. customdried