Reaction #2329085

ord-185634b09ebd45c789125ecf23fc3ac1

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Extractionthe mixture was extracted with ethyl acetate
  2. 2
    WashThe organic layer was washed with saturated brine
  3. 3
    Dryingdried over anhydrous sodium sulfate
  4. 4
    OtherThe residue obtained by evaporation of the solvent under reduced pressure
  5. 5
    Otherwas purified by column chromatography on silica gel (n-hexane:ethyl acetate=1:2)

Procedure

Piperidine (0.081 g, 0.950 mmol) and potassium carbonate (0.380 g, 2.77 mmol) were added to a solution of 3-chlor-1-[4-(2-fluoro-4-nitrophenyl)piperazin-1-yl]propan-1-one (compound of Reference Example 58; 0.250 g, 0.790 mmol) in anhydrous N,N-dimethylformamide (6 ml), and the mixture was stirred at room temperature for 10 hours. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The residue obtained by evaporation of the solvent under reduced pressure was purified by column chromatography on silica gel (n-hexane:ethyl acetate=1:2) to give the title compound (0.120 g, 41%) as a yellow solid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07671058B2uspto-grants-2010_03