HRID748056
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
- -78 °C
PROCEDURE
实验过程
To a stirred solution of 1-(4-fluorobenzyl)-1H-1,2,4-triazole (0.500 g, 2.82 mmol) in THF (30 mL) at −78° C. was added a solution of n-butyllithium (2.5M in hexanes, 1.1 mL, 2.9 mmol) dropwise. The mixture was stirred at −78° C. for 1.5 h, then 2-ethylbutyraldehyde (0.42 mL, 3.4 mmol) was added. The solution was slowly warmed to room temperature and stirred i 8 h. It was then quenched with saturated aqueous NH4Cl and extracted twice with EtOAc. The organic extracts were dried (MgSO4), filtered, concentrated in vacuo and purified by column chromatography (SiO2, EtOAc/hexane, 1:1) to yield an oil in 47% yield.
WORKUP
后处理
- temperatureThe solution was slowly warmed to room temperature
- stirringstirred i 8 h
- customIt was then quenched with saturated aqueous NH4Cl
- extractionextracted twice with EtOAc
- dry with materialThe organic extracts were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- custompurified by column chromatography (SiO2, EtOAc/hexane, 1:1)
- customto yield an oil in 47% yield