反应详情

Diethyl azodicarboxylate (40% in toluene, 2.5 ml, 5.5 mmol) was added to the mixture of N-Boc-4-hydroxypiperidine (1.0 g, 5.0 mmol), N-hydroxyphthalimide (816 mg, 5.0 mmol) and triphenylphosphine (1.3 g, 5.0 mmol) in THF (10 ml) at 0° C. and stirred at room temperature for 1.5 hours. The solvent was evaporated under reduced pressure and the residue was diluted with ethyl acetate and washed with water and brine, dried (MgSO4) and evaporated under reduced pressure. The residue was purified by column chromatography on silica (EtOAc/Hexanes 30/70-70/30) to give tert-butyl 4-(1,3-dioxoisoindolin-2-yloxy)piperidine-1-carboxylate (1.37 g, 80%).

1. customThe solvent was evaporated under reduced pressure
2. additionthe residue was diluted with ethyl acetate
3. washwashed with water and brine
4. dry with materialdried (MgSO4)
5. customevaporated under reduced pressure
6. customThe residue was purified by column chromatography on silica (EtOAc/Hexanes 30/70-70/30)