HRID376155
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
PROCEDURE
实验过程
65 g (0.33 tool) of benzyl 4-hydroxybutyrate and 260 mg of copper powder are charged to 120 ml of cyclohexane and the mixture is heated to reflux. Then a mixture of 38.7 ml (0.37 mol) of ethyl diazoacetate and 300 ml of cyclohexane are added, whereupon evolution of N2 ensues. The reaction mixture is stirred for 4 hours under reflux and then for 4 hours at room temperature, filtered over a glass fibre filter and concentrated by evaporation. The residue is chromatographed on silica gel with hexane/ethyl acetam 4:1, giving benzyl 4-ethoxycarbonylmethoxybutyrate as a colourless liquid.
WORKUP
后处理
- temperaturethe mixture is heated to reflux
- temperatureunder reflux
- waitfor 4 hours at room temperature
- filtrationfiltered over a glass fibre
- filtrationfilter
- concentrationconcentrated by evaporation
- customThe residue is chromatographed on silica gel with hexane/ethyl acetam 4:1