Reaktion #76559

ord-d335b0ed4e1f44deb4d7c29830e9fead

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture was filtered through a layer of Celite®
  2. 2
    Filtrationfilter agent
  3. 3
    Waschenthe filter cake was rinsed well with methanol
  4. 4
    workup.ADDITIONThe filtrate was treated with charcoal
  5. 5
    Einengenconcentrated under vacuum
  6. 6
    Sonstigeto provide a fluffy pale green solid
  7. 7
    SonstigeThis material was triturated with acetonitrile

Vorschrift

7-Methyl-3-nitro-4-quinolinol (11.8 g, 58 mmol), methanol (about 300 mL), ammonium hydroxide (50 mL), and palladium on carbon (1 g of 10%) were combined. The mixture was placed on a Parr apparatus under a 35-40 psi (2.4-2.8 Kg/cm2) hydrogen atmosphere for about 1 hour. The reaction mixture was filtered through a layer of Celite® filter agent and the filter cake was rinsed well with methanol. The filtrate was treated with charcoal and then concentrated under vacuum to provide a fluffy pale green solid. This material was triturated with acetonitrile to provide 8.5 g of 3-amino-7-methyl-4-quinolinol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06703402B2uspto-grants-2004_03