反应详情

温度

-78 °C

To a solution of N-(tert-butyl)benzenesulfonamide (569 mg, 0.00267 mol) in ether (10 mL, 0.1 mol) was added 1.7 M of tert-butyllithium in pentane (4.7 mL) under nitrogen at −78° C. The mixture was stirred at −78° C. for 15 minutes, then at 0° C. for 1 hour. The reaction mixture then was cooled down to −78° C. again and a solution of 1-{[1-(4-chlorophenyl)cyclopropyl]carbonyl}pyrrolidin-3-one (640 mg, 0.0024 mol) in ether was added. After stirring for 2 hours, the reaction mixture was quenched with saturated NH4Cl aqueous solution and then extracted with EtOAc. The combined organic layer was washed with brine, dried over MgSO4 and concentrated. The crude product was purified using Combiflash eluting with 30% AcOEt in hexanes to afford the desired product. LC/MS (M+H+) 478.0.

1. waitat 0° C. for 1 hour
2. temperatureThe reaction mixture then was cooled down to −78° C. again
3. stirringAfter stirring for 2 hours
4. customthe reaction mixture was quenched with saturated NH4Cl aqueous solution
5. extractionextracted with EtOAc
6. washThe combined organic layer was washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated
9. customThe crude product was purified
10. washeluting with 30% AcOEt in hexanes