Reaktion #161026

ord-12b502c590f642ac9c7cef359ce9cca9

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe reaction solution was concentrated under reduced pressure
  2. 2
    workup.ADDITIONToluene was added to the obtained residue, it
  3. 3
    workup.DISTILLATIONwas distilled off under reduced pressure three times, and acetic anhydride
  4. 4
    Sonstigewas removed by azeotropic distillation

Vorschrift

After a suspension of 631 mg (1.54 mmol) of 1-[[[4-(4-propylpiperazin-1-yl)phenyl]carbonyl]amino]cyclohexanecarboxylic acid hydrochloride in 18 ml of acetic anhydride was stirred at 100° C. for 1 hour, the reaction solution was concentrated under reduced pressure. Toluene was added to the obtained residue, it was distilled off under reduced pressure three times, and acetic anhydride was removed by azeotropic distillation to obtain 500 mg (83%) of the title compound.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829209B2uspto-grants-2014_09