Reaktion #435868

ord-c78bc65b881f477a8b50c4a0f7d59f98

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter having been cooled with ice
  2. 2
    SonstigeAfter the reaction
  3. 3
    Filtrationthe solution was filtrated through Celite
  4. 4
    workup.DISTILLATIONthe solvent was then distilled off
  5. 5
    SonstigeThen, the residue was purified through silica gel column chromatography (chloroform/methanol)
  6. 6
    workup.ADDITIONtreated with hydrochloric acid

Vorschrift

The compound (212 mg) obtained in Example 87-5 was dissolved in methanol (10 ml). After having been cooled with ice, the solution was added with a suspension of 10% palladium-carbon (105 mg) in ethanol (3.0 ml). After having been subjected to hydrogen displacement, the mixture was stirred under a hydrogen atmosphere at room temperature for 3 hours. After the reaction, the solution was filtrated through Celite and the solvent was then distilled off. Then, the residue was purified through silica gel column chromatography (chloroform/methanol) and treated with hydrochloric acid, thereby obtaining hydrochloride (43.1 mg) of the subject compound as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07176227B2uspto-grants-2007_02