反应详情

3.56 g (148.5 mmol) of sodium hydride is added to 24.03 g (123.74 mmol) of 2-(4-hydroxyphenyl)-propanoic acid ethyl ester in 400 ml of dimethylformamide and stirred for 1 hour at room temperature (under nitrogen). 34.35 g (371.22 mmol) of epichlorohydrin is added and then heated for 24 hours at 70° C. It is cooled in an ice bath to 0° C. and 800 ml of water is carefully added. Then, it is extracted twice with 350 ml of ether each. The combined ether phases are washed once with 300 ml of water, dried on magnesium sulfate and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel (mobile solvent: hexane/ethyl acetate=20:1)

1. temperatureheated for 24 hours at 70° C
2. temperatureIt is cooled in an ice bath to 0° C.
3. extractionThen, it is extracted twice with 350 ml of ether each
4. washThe combined ether phases are washed once with 300 ml of water
5. customdried on magnesium sulfate
6. concentrationconcentrated by evaporation in a vacuum
7. customThe residue is chromatographed on silica gel (mobile solvent: hexane/ethyl acetate=20:1)