Reaktion #625843
ord-f3b5f33e2aa04103be774d913a3b03ab
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1FiltrationThe reaction mixture was then filtered
- 2Einengenthe filtrate was concentrated
- 3workup.DISSOLUTIONThe residue was dissolved in EtOAc
- 4Waschenthe organic layer was washed with water and brine solution
- 5TrocknenThe organic layer was dried over Na2SO4
- 6Filtrationfiltered
- 7Einengenconcentrated
- 8SonstigeThe crude material was purified by chromatography on 230-400 mesh silica gel eluting with 30% EtOAc-hexane
Vorschrift
To a stirred solution of piperidine-2-methanol (12; 6 g, 52.09 mmol) in dimethylformamide (DMF, 50 mL) were added successively K2CO3 (10.78 g, 78.14 mmol) and benzyl bromide (6.85 mL, 57.30 mmol) at 0° C. and the mixture stirred at rt for 16 hours. The reaction mixture was then filtered and the filtrate was concentrated. The residue was dissolved in EtOAc and the organic layer was washed with water and brine solution. The organic layer was dried over Na2SO4, filtered and concentrated. The crude material was purified by chromatography on 230-400 mesh silica gel eluting with 30% EtOAc-hexane to provide compound 13.