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 13.8 parts of 1H-1,2,4-triazole, 18.7 parts of 1-bromo-4-methoxybenzene, 5 parts of potassium carbonate, 0.5 parts of copper (I)chloride and 90 parts of N,N-dimethylformamide is stirred and refluxed for 2 days. The reaction mixture is cooled and poured onto water. The product is extracted twice with benzene. The combined extracts are washed with water, dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions are collected and the eluent is evaporated. The residue is triturated in 2,2'-oxybispropane. The product is filtered off and dried, yielding 7.8 parts (44.5%) of 1-(4-methoxyphenyl)-1H-1,2,4-triazole; mp. 99.4° C.
WORKUP
后处理
- temperaturerefluxed for 2 days
- temperatureThe reaction mixture is cooled
- additionpoured onto water
- extractionThe product is extracted twice with benzene
- washThe combined extracts are washed with water
- customdried
- filtrationfiltered
- customevaporated
- customThe residue is purified by column-chromatography over silica gel
- customThe pure fractions are collected
- customthe eluent is evaporated
- customThe residue is triturated in 2,2'-oxybispropane
- filtrationThe product is filtered off
- customdried