反应详情

To a solution of ethyl(2S)-2-ethoxy-3-[4-(2-{ethyl[4-(trifluoromethoxy)benzyl]amino}-2-oxoethoxy)phenyl]propanoate (0.560 g, 1.13 mmol) in THF (50 mL) was added aqueous 0.10 M LiOH (25 mL) and the solution was stirred at room temperature overnight. After neutralisation with 5% HCl, the solvent volume was reduced in vacuo and the remaining aqueous phase was acidified with 5% HCl and extracted with ethyl acetate (2×50 mL). The combined organic phase was washed with brine (50 mL), dried over Na2SO4, and concentrated in vacuo. Purification on a prepacked column of silica gel (Isolute® SPE Column, 10 g/70 mL) with ethyl acetate as the eluent afforded 0.457 g (87%) of a colourless oil.

1. extractionextracted with ethyl acetate (2×50 mL)
2. washThe combined organic phase was washed with brine (50 mL)
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. customPurification on a prepacked column of silica gel (Isolute® SPE Column, 10 g/70 mL) with ethyl acetate as the eluent