HRID881982
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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
To solution of 1,3-dibromobenzene (84 g, 356 mmol) in DMF (700 ml) was added 1,2,3-1H-triazole (30 g, 427 mmol), Cul (6.8 g, 35.6 mmol), Iron(III) acetylacetonate (38 g, 107 mmol) and cesium carbonate (231 g, 712 mmol). The resulting mixture was heated to 120° C. under a nitrogen atmosphere overnight. After cooling to room temperature the reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The obtained residue was purified using normal phase chromatography eluting with petroleum ether containing 20% ethyl acetate to give 2-(3-bromophenyl)-2H-1,2,3-triazole (28 g) and 1-(3-bromophenyl)-1H-1,2,3-triazole (11 g) as the pure isomers.
WORKUP
后处理
- temperatureAfter cooling to room temperature the reaction mixture
- filtrationwas filtered
- concentrationthe filtrate was concentrated under reduced pressure
- customThe obtained residue was purified
- washeluting with petroleum ether containing 20% ethyl acetate