Reaktionsgleichung
[N+:1]([C:4]1[C:17]2[C:16](=[O:18])[C:15]3[C:10](=[C:11]([N+:20]([O-])=O)[CH:12]=[CH:13][C:14]=3[OH:19])[C:9](=[O:23])[C:8]=2[C:7]([OH:24])=[CH:6][CH:5]=1)([O-])=O.[OH-].[Na+].[H][H]>[C].[Pd]>[NH2:1][C:4]1[C:17]2[C:16](=[O:18])[C:15]3[C:10](=[C:11]([NH2:20])[CH:12]=[CH:13][C:14]=3[OH:19])[C:9](=[O:23])[C:8]=2[C:7]([OH:24])=[CH:6][CH:5]=1Komponenten
Versuchsvorschrift
A 500 ml. electromagnetically stirred glass reactor was charged with 5.0 g (0.0151 mole) of 1,5-dinitro-4,8-dihydroxyanthraquinone, 100 g of a 4% aqueous solution of sodium hydroxide and 0.25 g of 5% palladium-carbon. The inside of the reactor was purged with hydrogen, and the 1,5-dinitro-4,8-dihydroxyanthraquinone was hydrogenated at 50° C. with stirring. In 5 hours, 0.0906 mole of hydrogen was absorbed, whereupon the reaction was stopped. The reaction mixture was filtered to separate the catalyst. The filtrate was oxidized with air with stirring at 20° to 30° C. for 2 hours, and then neutralized with 20% sulfuric acid to a pH of 2-3. The crystals precipitated were filtered, washed with water, and dried to afford 4.0 g of 1,5-diamino-4,8-dihydroxyanthraquinone in a yield of 97.8%.
Aufarbeitung
- customThe inside of the reactor was purged with hydrogen
- customwas hydrogenated at 50° C.
- filtrationThe reaction mixture was filtered
- customto separate the catalyst
- stirringwith stirring at 20° to 30° C. for 2 hours
- customThe crystals precipitated
- filtrationwere filtered
- washwashed with water
- customdried
Quellen und Nachweise
- ORD-Eintrag
- ord-d2442c56e3b1499e9c4c1a15a419fa06
- Quelldatensatz
- uspto-grants-1977_09
- Patentnummer
- US04046785
Verknüpfte Notizen
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