反应详情

A solution of 0.795 g of 2-methyl-2-(tetrahydro-pyran-4-yl)-propionic acid ethyl ester in 3 ml of ethanol is admixed with 3 ml of a 40% aqueous potassium hydroxide solution and then heated to reflux. After 4 hours, the reaction mixture is cooled to room temperature and the ethanol removed in vacuo. The remaining aqueous solution is acidified (pH 2-3) with 4M HCl and then extracted with tert-butyl methyl ether (2×). The combined organic layers are washed with water and brine, dried over sodium sulphate and concentrated by evaporation to provide the crude title compound as a yellow solid. Rf=0.10 (1:3 EtOAc-heptane).

1. temperatureheated to reflux
2. customthe ethanol removed in vacuo
3. extractionextracted with tert-butyl methyl ether (2×)
4. washThe combined organic layers are washed with water and brine
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated by evaporation