反应详情

温度

14 °C

A solution of tert-butyl 4-formylpiperidine-1-carboxylate (50.0 g, 234 mmol) in MeOH (200 mL) and water (200 mL) was cooled in an ice-bath and then hydroxylamine hydrochloride (19.5 g, 272 mmol) and sodium carbonate (12.4 g, 117 mmol) were added. The resulting mixture was stirred at 13-15° C. overnight. The solution was concentrated in vacuo to an aqueous suspension, which was extracted with EtOAc. The organic extract was washed with 100 mL brine, dried (MgSO4), filtered, concentrated to provide tert-butyl 4-((hydroxyimino)methyl)piperidine-1-carboxylate (53.1 g, 99.2% yield) as a white crystalline solid.

1. concentrationThe solution was concentrated in vacuo to an aqueous suspension, which
2. extractionwas extracted with EtOAc
3. extractionThe organic extract
4. washwas washed with 100 mL brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated