Reaktion #1369326

ord-01b5a3a50b7c4dd58edbb49db5ad8b3f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with chloroform
  2. 2
    WaschenThe extract was washed with saturated brine
  3. 3
    Trocknendried over anhydrous sodium sulfate
  4. 4
    SonstigeThe solvent was evaporated
  5. 5
    Sonstigethe obtained residue was purified by silica gel column chromatography (

Vorschrift

A solution of N-(4-chloromethylphenylmethyl) acetamide (0.85 g), 1-(pyridin-4-yl)piperazine (0.64 g) and potassium carbonate (0.81 g) in dimethylformamide (10 ml) was stirred at 60-70° C. for 5 hr. The reaction mixture was poured into water and extracted with chloroform. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (developing solvent; chloroform:methanol=9:1)to give a yellow solid(0.6 g). The obtained yellow solid was crystallized from ethyl acetate-methanol to give the title compound (0.37 g) as white crystals, m.p.=164-166° C.

Quelle

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