HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 4-Methoxy-2,3,5-trimethylpyridine 1-oxide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Methanol | HCID 887 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Edukt | 4-Nitro-2,3,5-trimethylpyridine, 1-oxide | HCID 11217611 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 4-Methoxy-2,3,5-trimethylpyridine 1-oxide | HCID 10702237 | — |
Reaktionsschritte
22.6 g of sodium are dissolved in 4 1 of methanol under argon. 120 g of 2,3,5-trimethyl-4-nitropyridine 1-oxide are then added portionwise thereto and the solution is left to boil under reflux overnight. The pH is adjusted to 7 by means of 5N hydrogen chloride in ethyl acetate while cooling and the mixture is then evaporated in vacuo. The residue is taken up in 1.5 1 of methylene chloride, the solution is filtered throuqh siliceous earth, which is rinsed with 0.5 1 of methylene chloride, the combined filtrates are evaporated in vacuo and the residue is crystallized from petroleum ether. There is obtained 4-methoxy-2,3,5-trimethylpyridine 1-oxide of melting point 48°-50°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04766133 |
| Quelldatensatz | uspto-grants-1988_08 |
| ORD ID | ord-518b8ecebb294c6991c42d564bd64b1a |
| Quellennotiz | uspto-grants-1988_08 |