Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Ethyl acetylphenylacetate | HCID 95389 | — |
| Edukt | HCID 178418311 | HCID 178418311 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Tributylamine | HCID 7622 | — |
| Produkt | HCID 178421927 | HCID 178421927 | — |
Reaktionsschritte
A solution of 3.8 g 1,2,4-triazol-3-amine and 6 g ethyl 3-oxo-2-phenylbutanoate is suspended in a mixture of 32 ml DMF and 32 ml N,N-dibutylbutan-1-amine and heated by microwave irradiation to 180° C. for 10 h. The reaction mixture is diluted with water and dichloromethane, the phases separated, the aqueous layer extracted twice with dichloromethane, the combined organic layers are dried over Na2SO4 and concentrated to give the crude product. The crude product is purified by column chromatography (silica gel, dichloromethane/methanol).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07776864B2 |
|---|
| Quelldatensatz | uspto-grants-2010_08 |
|---|
| ORD ID | ord-637348febe354317b72ed4226981a1e6 |
|---|
| Quellennotiz | uspto-grants-2010_08 |
|---|