HRID2364593
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
A mixture of 4-iododibenzo[b,d]furan (5 g, 17.00 mmol), 1H-1,2,4-triazole (3.52 g, 51.0 mmol), CuI (0.162 g, 0.850 mmol), N1,N2-dimethylcyclohexane-1,2-diamine (0.537 mL, 3.40 mmol) and K3PO4 (7.58 g, 35.7 mmol) in DMF (50 mL) was heated at 140° C. for 48 h. After cooling to room temperature, the reaction mixture was filtered through a short plug of Celite®, and the solid was washed with DCM. The combined filtrate was evaporated and purified by column chromatography on silica gel with DCM as eluent to yield 1-(dibenzo[b,d]furan-4-yl)-1H-1,2,4-triazole (2.4 g, 60%) as white powder.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- filtrationthe reaction mixture was filtered through a short plug of Celite®
- washthe solid was washed with DCM
- customThe combined filtrate was evaporated
- custompurified by column chromatography on silica gel with DCM as eluent