Reaktion #10039

ord-c3fa110c818b49349c5d166723b662c8

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITto stand overnight at the same temperature
  2. 2
    Extraktionwas then extracted
  3. 3
    SonstigeThe organic layer was separated from the aqueous layer, which
  4. 4
    Waschenwas washed with water (10 mL)
  5. 5
    SonstigeThe solvent of the organic layer was removed by distillation under reduced pressure

Vorschrift

Potassium thioacetate (677 mg) was added to a solution of methyl (2S,4R)-4-methylsulfonyloxy-1-methyl-2-pyrrolidinecarboxylate (609 mg) obtained from Reference example 4 in ethanol/water (9:1) (6 ml), and the resulting mixture was stirred at 80° C. for 3 hours, and then the mixture was allowed to stand overnight at the same temperature. Ethyl acetate (20 mL) and 10% aqueous sodium chloride solution (10 mL) were added to the reaction mixture, which was then extracted. The organic layer was separated from the aqueous layer, which was washed with water (10 mL). The solvent of the organic layer was removed by distillation under reduced pressure to give the title compound (543 mg, yield 97%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091363B2uspto-grants-2006_08