反应详情

To a solution of 108 (41.1 g, 287.0 mmol), imidazole (29.31 g, 430.6 mmol), and DMAP (3.507 g, 28.70 mmol) in DMF (100 mL) was added slowly tert-butylchlorodimethylsilane (54.08 g, 358.8 mmol) and the reaction was stirred at RT for 18 h. Water was added and mixture was extracted with Et2O. The organic layer was dried, filtered, and concentrated. The resulting residue was purified by passing through a SiO2 plug eluting with an EtOAc/hexane gradient (10 to 50% EtOAc) to afford 56.93 g (77.04%) of (S)-2-(tert-butyldimethylsilyloxy)-1-(pyrrolidin-1-yl)propan-1-one (110).

1. extractionmixture was extracted with Et2O
2. customThe organic layer was dried
3. filtrationfiltered
4. concentrationconcentrated
5. customThe resulting residue was purified
6. washeluting with an EtOAc/hexane gradient (10 to 50% EtOAc)