反应详情

To a solution of tert-butyl 4-(2,5-dibromopentanamido)piperidine-1-carboxylate (2.21 g, 5.00 mmol) dissolved in DMF (10 mL) was added 60% sodium hydride (0.220 g, 5.5 mmol). The reaction was allowed to stir for 2 hours and then concentrated under vacuum. The resulting material was diluted with water and EtOAc. The organic layer was separated and the aqueous layer washed with EtOAc. The combined organic layers were dried with MgSO4 and concentrated. The residue was purified over silica gel (2:1 hexanes:EtOAc) to give tert-butyl 3-bromo-2-oxo-1,4′-bipiperidine-1′carboxylate (1.35 g, 75%) as a white solid.

1. concentrationconcentrated under vacuum
2. additionThe resulting material was diluted with water and EtOAc
3. customThe organic layer was separated
4. washthe aqueous layer washed with EtOAc
5. dry with materialThe combined organic layers were dried with MgSO4
6. concentrationconcentrated
7. customThe residue was purified over silica gel (2:1 hexanes:EtOAc)