Reaktion #625843

ord-f3b5f33e2aa04103be774d913a3b03ab

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was then filtered
  2. 2
    Einengenthe filtrate was concentrated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in EtOAc
  4. 4
    Waschenthe organic layer was washed with water and brine solution
  5. 5
    TrocknenThe organic layer was dried over Na2SO4
  6. 6
    Filtrationfiltered
  7. 7
    Einengenconcentrated
  8. 8
    SonstigeThe 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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08865741B2uspto-grants-2014_10