Reaktion #1369316

ord-e710ec5cf84940cf8a881d0dfcf6e632

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe solution was refluxed
  2. 2
    Temperaturunder heating for 12.5 hr
  3. 3
    Extraktionthe mixture was extracted with ethyl acetate
  4. 4
    WaschenThe extract was washed with saturated brine
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    SonstigeThe solvent was evaporated
  7. 7
    Sonstigethe obtained residue was crystallized from diisopropyl ether

Vorschrift

N-(4-((4-(Pyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide (4.0 g) was dissolved in 10% hydrochloric acid (50 ml) and the solution was refluxed under heating for 12.5 hr. To the reaction mixture was added 10% aqueous sodium hydroxide solution to make it alkaline, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was crystallized from diisopropyl ether to give the title compound (2.2 g) as pale-yellow crystals, m.p.=70-72° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06455528B1uspto-grants-2002_09