反应详情

温度

0 °C

A solution of lithium hydroxide (1 g, 22 mmol) in water (44 ml) was added dropwise to a solution of methyl 2-(1-(3-(trifluoromethyl)phenylsulfonyl)piperidin-2-yl)acetate (4.38 g, 12 mmol) in tetrahydrofuran (176 ml) while stirring at 0° C. The mixture was stirred for 16 h at 25° C. The solvent was removed under vacuum, the residue dissolved in water and washed with diethyl ether. The aqueous phase was carefully acidified with citric acid solution (10%) and extracted with ethyl acetate. This organic phase was washed with water and saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated to small volume under vacuum. The crude product was used in the next stage with no further purification. Yield: 90%

1. stirringThe mixture was stirred for 16 h at 25° C
2. customThe solvent was removed under vacuum
3. dissolutionthe residue dissolved in water
4. washwashed with diethyl ether
5. extractionextracted with ethyl acetate
6. washThis organic phase was washed with water and saturated sodium chloride solution
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated to small volume under vacuum
10. customThe crude product was used in the next stage with no further purification