HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diethyl Ether → Methyl 3-amino-4-methylthiophene-2-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diethyl Ether | HCID 3283 | — |
| Edukt | Hydroxyamine hydrochloride | HCID 443297 | — |
| Edukt | Methyl tetrahydro-4-methyl-3-oxo-2-thiophenecarboxylate | HCID 10487456 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Methyl 3-amino-4-methylthiophene-2-carboxylate | HCID 123584 | — |
Reaktionsschritte
2-Methoxycarbonyl-4-methyl-3-oxotetrahydrothiophene (l.74 g) was dissolved in acetonitrile (13 ml) and the resulting solution was brought to the boil. To this was added hydroxylamine hydrochloride (0.69 g) and the mixture was refluxed for 5 hours. The reaction mixture was cooled in ice and dry ether (50 ml) added whereby a sticky precipitate was produced which was filtered off with the aid of kieselguhr. The kieselguhr was slurried with water and filtered, and the filtrate was basified with ammonia and extracted with ether (2 ×). The combined extracts were dried over sodium sulphate, filtered and evaporated to give the title compound, 1.lg (64%) mp 82°-83°.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04847386 |
| Quelldatensatz | uspto-grants-1989_07 |
| ORD ID | ord-f762d8d93bd8435790262ce47ec8b218 |
| Quellennotiz | uspto-grants-1989_07 |