HRID244669
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
- 20 °C
PROCEDURE
实验过程
To a solution of ethyl 1H-pyrazole-3-carboxylate (0.77 g) (available from ABCR) in acetonitrile (30 ml) was added cesium carbonate (1.79 g) and the mixture stirred for 5 min when 1-fluoro-2-iodoethane (0.96 g) was added and the mixture stirred at 20° C. for 18 h. The mixture was evaporated and the residue taken up in water (30 ml) and DCM (30 ml) separated by hydrophobic frit and concentrated to ˜5 ml, placed on an SPE cartridge (50 g silica) and eluted with a gradient of ethyl acetate in cyclohexane to give the Ethyl 1-(2-fluoroethyl)-1H-pyrazole-5-carboxylate (0.42 g) as a colourless oil.
WORKUP
后处理
- additionwas added
- customThe mixture was evaporated
- customDCM (30 ml) separated by hydrophobic frit
- concentrationconcentrated to ˜5 ml
- washeluted with a gradient of ethyl acetate in cyclohexane