Reaktion #44099

ord-966ccbaf97cf4e198a4ec66239090793

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthen concentrated
  2. 2
    workup.ADDITIONWater (30 vol) was added
  3. 3
    Extraktionthe solution was extracted with ethyl acetate (3×20 vol)
  4. 4
    Extraktionthen extracted with dichloromethane (5×40 vol)
  5. 5
    SonstigeThe combined organic extracts were dried
  6. 6
    Sonstigeevaporated

Vorschrift

To a solution of 1,1-dimethylethyl 4-(2-methyl-5-quinolinyl)-1-piperazinecarboxylate in 2-propanol (3 vol) was added dropwise hydrochloric acid (37%, 3 vol). The mixture was stirred at 40° C. for 1.5 hours then concentrated. Water (30 vol) was added and the solution was extracted with ethyl acetate (3×20 vol). The aqueous layer was basified with an aqueous sodium carbonate solution then extracted with dichloromethane (5×40 vol). The combined organic extracts were dried and evaporated to give the title compound as an off-white solid (80% th, 2 steps).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07732600B2uspto-grants-2010_06