反应详情

65 g (0.33 mol) 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 acetate 4:1, giving benzyl 4-ethoxycarbonylmethoxybutyrate as a colourless liquid.

1. temperaturethe mixture is heated to reflux
2. temperatureunder reflux
3. waitfor 4 hours at room temperature
4. filtrationfiltered over a glass fibre
5. filtrationfilter
6. concentrationconcentrated by evaporation
7. customThe residue is chromatographed on silica gel with hexane/ethyl acetate 4:1