Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sulfapyridine | HCID 5336 | — |
| Edukt | (2-Hydroxyphenyl)acetic acid | HCID 11970 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Lösungsmittel | Hydrochloric Acid | HCID 313 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | Homosulphasalazine | HCID 192035 | — |
Reaktionsschritte
12 g sulfapyridine was dissolved with cooling to 0° C. in 40 ml water and 12 ml conc. hydrochloric acid. 3.5 g sodium nitrite in 20 ml water was added to the sulfapyridine solution during about 15 minutes with stirring and cooling. The diazonium salt solution was added to 7.6 g 2-hydroxy-benzeneacetic acid and 7 g sodium hydroxide in 50 ml water at 0°-10° C. After stirring for 1.5 h the solution was acidified by hydrochloric acid. The precipitating product was filtered off and washed with water. Yield 18.1 g. The product was dissolved in acetic acid and treated with 5 g decolourizing coal. The solution was filtered and evaporated in vacuum. This was repeated once, a pure product being obtained, which during partial melting at about 135° C. was converted into another crystal modification of melting point 185°-187° C. with decomposition.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04628083 |
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| Quelldatensatz | uspto-grants-1986_12 |
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| ORD ID | ord-e64b64b6fc094a41b0a7b76a6ba35ead |
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| Quellennotiz | uspto-grants-1986_12 |
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