反应详情

温度

60 °C

To a stirred solution of rac {1-[(2R,3S,4R,5S)-3-(3-Chloro-2-fluoro-phenyl)-4-(4-chloro-2-fluoro-phenyl)-4-cyano-5-(2,2-dimethyl-propyl)-pyrrolidine-2-carbonyl]-piperidin-4-yl}-acetic acid methyl ester (556 mg, 0.92 mmol) in methanol (8 mL), LiOH.H2O (Aldrich, 80 mg) in 1 mL of water was added. The mixture was stirred at 60° C. overnight. The reaction was quenched with addition of water. The mixture was filtered and the filtrate was concentrated to removed methanol. The aqueous layer was washed with EtOAc (2×5 mL) and acidified with 3N HCl. The mixture was then extracted with EtOAc (3×6 mL). The extracts were combined and dried over sodium sulfate and concentrated to give a white solid. 649 mg.

1. customThe reaction was quenched with addition of water
2. filtrationThe mixture was filtered
3. concentrationthe filtrate was concentrated
4. customto removed methanol
5. washThe aqueous layer was washed with EtOAc (2×5 mL)
6. extractionThe mixture was then extracted with EtOAc (3×6 mL)
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated
9. customto give a white solid