Reaktion #11954
ord-556b3489715040888ff745b81e37a366
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeAfter the completion of the reaction
- 2Sonstigethe solid was removed
- 3Filtrationfilter
- 4Einengenthe filtrate was concentrated
- 5workup.DISSOLUTIONThe residue was dissolved in chloroform
- 6Waschenwashed with 1 mol/l aqueous solution of sodium hydroxide and saturated brine
- 7TrocknenThe solution was dried over anhydrous sodium sulfate
- 8SonstigeThe solvent was removed by distillation
- 9Sonstigethe 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.