Reaktion #481120
ord-a1899ec0f0ff49a7972894c2a7d161de
Reaktionsgleichung
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1FiltrationThe reaction mixture was filtered through a layer of Celite®
- 2Filtrationfilter agent
- 3Waschenthe filter cake was rinsed well with methanol
- 4workup.ADDITIONThe filtrate was treated with charcoal
- 5Einengenconcentrated under vacuum
- 6Sonstigeto provide a fluffy pale green solid
- 7SonstigeThis 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.