HRID748058
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
PROCEDURE
实验过程
To a stirred solution of 2-ethyl-1-[1-(4-fluorobenzyl)-1H-1,2,4-triazol-5-yl]butan-1-ol (0.459 g, 1.42 mmol) in DMF (10 mL) was added sodium azide (0.277 g, 4.26 mmol) and the mixture was heated to reflux for 3 h. After cooling, the reaction mixture was diluted with H2O and extracted with EtOAc twice. The organic extracts were dried (MgSO4), filtered, concentrated in vacuo and purified by column chromatography (SiO2, EtOAc/hexane, 1:9) to yield a clear oil in 67% yield.
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureto reflux for 3 h
- temperatureAfter cooling
- extractionextracted with EtOAc twice
- dry with materialThe organic extracts were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- custompurified by column chromatography (SiO2, EtOAc/hexane, 1:9)
- customto yield a clear oil in 67% yield