Reaktion #1818188

Reaktionsgleichung

hydrogen

sodium hydroxide

5-nitrotetrahydroanthraquinone

dipropylene glycol

→

1-aminoanthraquinone

Ausbeute 87.3%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeat 120° C.
2. 2
   SonstigeHydrogen was absorbed in the starting 5-nitro compound in an amount of 2mols per mol of the 5-nitro compound
3. 3
   FiltrationAfter completion of the hydrogenation, the resultant solution was subjected to filtration under hot conditions at 120° to 130° C.
4. 4
   Sonstigeto remove the catalyst
5. 5
   workup.ADDITIONTo the resultant filtrate was added 350 grams of water for dilution
6. 6
   Sonstigeto obtain crystals which
7. 7
   Sonstigewere separated by filtration
8. 8
   Waschenwashed with water
9. 9
   Sonstigedried

Vorschrift

0.1 Gram of a 5% palladium on carbon catalyst and 10 grams of a 20% aqueous sodium hydroxide solution were added to a mixture of 12.8 grams of 5-nitrotetrahydroanthraquinone and 170 grams of dipropylene glycol in an autoclave, into which was fed hydrogen, until the pressure reached 25 kg/cm2, for hydrogenation of the 5-nitro compound at 120° C. with agitation. Hydrogen was absorbed in the starting 5-nitro compound in an amount of 2mols per mol of the 5-nitro compound. After completion of the hydrogenation, the resultant solution was subjected to filtration under hot conditions at 120° to 130° C. to remove the catalyst therefrom. To the resultant filtrate was added 350 grams of water for dilution to obtain crystals which were separated by filtration, washed with water and dried to yield 9.7 grams of 1-aminoanthraquinone having a purity of 96.7%.

Quelle