反应详情

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0 °C

A mixture of rac-(2R,3S,4R,5S)-3-(3-chloro-2-fluoro-phenyl)-4-(4-chloro-3-fluoro-phenyl)-4-cyano-5-(2,2-dimethyl-propyl)-pyrrolidine-2-carboxylic acid tert-butyl ester (0.6 g, 1.15 mmol) was cooled to 0° C., then conc. H2SO4 (2 mL) was added slowly. The reaction was stirred at RT for 2 hours. The mixture was then poured into ice and extracted with EtOAc. The organic phase was separated, dried over Na2SO4, filtered and solvent was removed under reduced pressure to yield a residue that was triturated with ethyl acetate/heptane and the precipitates were collected by filtration and washed with ether to yield the product rac-(2R,3S,4R,5S)-3-(3-chloro-2-fluoro-phenyl)-4-(4-chloro-3-fluoro-phenyl)-4-cyano-5-(2,2-dimethyl-propyl)-pyrrolidine-2-carboxylic acid (0.526 g, 98.1%) as a white solid. HRMS (ES+) m/z Calcd for C23H22Cl2F2N2O2S+H [(M+H)+]: 467.1099. found: 467.1097.

1. additionThe mixture was then poured into ice
2. extractionextracted with EtOAc
3. customThe organic phase was separated
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customsolvent was removed under reduced pressure
7. customto yield a residue that
8. customwas triturated with ethyl acetate/heptane
9. filtrationthe precipitates were collected by filtration
10. washwashed with ether