反应详情

A solution of 0.069 g of benzyl 4-(3-fluoro-4-hydroxyphenyl)-3-hydroxypiperidine-1-carboxylate in 5 ml of acetone is admixed with 0.034 g of potassium carbonate and 0.019 ml of dimethyl sulphate. The reaction mixture is stirred at reflux over 5 hours, cooled and filtered through Hyflo. The filtercake is washed with 2×5 ml of acetone and the filtrate is concentrated by evaporation. The residue is taken up in 30 ml of tert-butyl methyl ether, washed with 10 ml of brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a colourless oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.38 (2:1 EtOAc-heptane); Rt=4.32.

1. temperatureat reflux over 5 hours
2. temperaturecooled
3. filtrationfiltered through Hyflo
4. washThe filtercake is washed with 2×5 ml of acetone
5. concentrationthe filtrate is concentrated by evaporation
6. washwashed with 10 ml of brine
7. dry with materialdried over sodium sulphate
8. concentrationconcentrated by evaporation