HRID443499

反应详情

EQUATION

反应方程式

HRID 443499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.1 g. of 3-(chloromethyl)-6-[3-(trifluoromethyl)phenyl]-1,2,4-triazolo[4,3-b]pyridazine and 0.40 g. of sodium methoxide in 50 ml. of ethanol is refluxed for 24 hours. The solvent is removed under reduced pressure and the residue is dissolved in dichloromethane. The solution is filtered through a column of hydrous magnesium silicate. The eluent is concentrated and hexane added to give 1.4 g. of the product of the Example as crystals, m.p. 149°-150° C. Recrystallization from dichloromethane-hexane gives 0.6 g. of white crystals, m.p. 149°-151° C.

WORKUP

后处理

  1. additionA mixture of 2.1 g
  2. customThe solvent is removed under reduced pressure
  3. dissolutionthe residue is dissolved in dichloromethane
  4. filtrationThe solution is filtered through a column of hydrous magnesium silicate
  5. concentrationThe eluent is concentrated
  6. additionhexane added
  7. customto give 1.4 g
  8. customRecrystallization from dichloromethane-hexane
  9. customgives 0.6 g