Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Urea | HCID 1176 | — |
| Edukt | 3,5-Dimethoxypyrazin-2-amine | HCID 20528923 | — |
| Edukt | Sodium Nitrite | HCID 23668193 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 178493795 | HCID 178493795 | — |
Reaktionsschritte
A solution of 2-amino-3,5-dimethoxypyrazine (0.02 mole) in 300 ml. of 6 M sulfuric acid at 0°-5° C. is treated with 0.022 mole sodium nitrite in 25 ml. of water at such a rate to insure that the temperature of the reaction mixture does not rise above 5° C. After standing 45 minutes at 0°-5° C., a little urea is added to destroy excess nitrous acid and the mixture then is treated with sodium hydroxide solution until strongly basic. The reaction mixture is warmed to 60° C. for one hour and then brought to pH 8.5. The mixture is concentrated to a third of the original volume and cooled in the refrigerator overnight. The product is separated by filtration and dried in vacuo, recrystallized from a suitable solvent to give 2-hydroxy-3,5-dimethoxypyrazine.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04343802 |
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| Quelldatensatz | uspto-grants-1982_08 |
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| ORD ID | ord-22a4062c69c940d6a699728656bd9c55 |
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| Quellennotiz | uspto-grants-1982_08 |
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