HRID443499
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionA mixture of 2.1 g
- customThe solvent is removed under reduced pressure
- dissolutionthe residue is dissolved in dichloromethane
- filtrationThe solution is filtered through a column of hydrous magnesium silicate
- concentrationThe eluent is concentrated
- additionhexane added
- customto give 1.4 g
- customRecrystallization from dichloromethane-hexane
- customgives 0.6 g