Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | 1-Nitroanthraquinone | HCID 6704 | — |
| Edukt | Sodium Azide | HCID 33557 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-Amino-4-hydroxyanthraquinone | HCID 8323 | — |
Reaktionsschritte
127 parts of 1-nitroanthraquinone are suspended at room temperature in 1000 parts of dimethyl formamide. To this suspension are then added 35 parts of sodium azide. The reaction mixture is then stirred for 8 hours at room temperature and, after addition of 1000 parts of a mixture of ice and water, filtered. The filter cake is washed with water and the moist product (28% paste) is added in the course of 2 hours to 1000 parts of conc. sulfuric acid, taking care that the temperature does not rise above 85° C. The suspension is then heated to 95° C., stirred for 3 hours at 95°-100° C. and, after the dropwise addition of 400 parts of ice-water, filtered hot. The filtrate is then poured into 4000 parts of ice-water and filtered. The filter cake is washed neutral with water, affording 100 parts of 1-amino-4-hydroxyanthraquinone.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04250102 |
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| Quelldatensatz | uspto-grants-1981_02 |
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| ORD ID | ord-d87c57f3e5364143ab8daa60d05569ed |
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| Quellennotiz | uspto-grants-1981_02 |
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