Reaktion #5187

ord-c4d16722518f4ca28ee5c209fc5afdcf

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITat room temperature for 1.5 hours
  2. 2
    Extraktionextracted with ethyl acetate
  3. 3
    WaschenThe extract was washed with an aqueous solution of sodium chloride
  4. 4
    Trocknendried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was then distilled off under reduced pressure

Vorschrift

13.3 ml of triethylamine and subsequently 7.4 ml of methanesulfonyl chloride were added, whilst ice-cooling, to a solution of 10 g of 4-hydroxy-1-methylpiperidine dissolved in 100 ml of dry tetrahydrofuran. The mixture was then stirred at 0° to 5° C. for 2 hours and then at room temperature for 1.5 hours, after which it was poured into an aqueous solution of sodium chloride and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then distilled off under reduced pressure, to afford 12.74 g of the title compound as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05242914uspto-grants-1993_09