Reaktion #11954

ord-556b3489715040888ff745b81e37a366

Lösungsmittel

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter the completion of the reaction
  2. 2
    Sonstigethe solid was removed
  3. 3
    Filtrationfilter
  4. 4
    Einengenthe filtrate was concentrated
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in chloroform
  6. 6
    Waschenwashed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine
  7. 7
    TrocknenThe solution was dried over anhydrous sodium sulfate
  8. 8
    SonstigeThe solvent was removed by distillation
  9. 9
    Sonstigethe residue was dried under reduced pressure

Vorschrift

The compound obtained in Example 17-1 (269.9 mg) was dissolved in carbontetrachloride (8 ml), and N-bromosuccinimide (252.6 mg) and azobisisobutylonitrile (22.1 mg) were added to the solution. The mixture was stirred for 6 hours at 70° C. After the completion of the reaction, the solid was removed using a glass filter and the filtrate was concentrated. The residue was dissolved in chloroform and washed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine. The solution was dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was dried under reduced pressure to obtain the title compound (363.3 mg) as pale yellow oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098215B2uspto-grants-2006_08