HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrazine hydrate (1:1) → N-{1-[3-(4-Nitrophenyl)-5-oxo-4,5-dihydro-1,2,4-triazin-6-yl]ethyl}acetamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Edukt | 4-Nitrobenzamidine hydrochloride | HCID 170625 | — |
| Edukt | Ethyl 3-acetamido-2-oxobutanoate | HCID 22245807 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | N-{1-[3-(4-Nitrophenyl)-5-oxo-4,5-dihydro-1,2,4-triazin-6-yl]ethyl}acetamide | HCID 135738336 | — |
Reaktionsbedingungen
| Temperatur | 20 °C |
|---|
Reaktionsschritte
7.30 g (7.09 ml, 145.82 mmol) of hydrazine hydrate are added dropwise to 24.50 g (121.5 mmol) of 4-nitrobenzenecarboximidamide hydrochloride from example 1A are in 250 ml of ethanol. The mixture is stirred for one hour at 20° C. After this time, 34.12 g (182.28 mmol) of ethyl 3-(acetylamino)-2-oxobutanoate from example 4A are added in ethanol, and the reaction mixture is stirred for 4 h at a bath temperature of 70–80° C., subsequently for 12 h at 20° C. The mixture is concentrated and the residue is purified by flash chromatography (eluent: ethyl acetate, subsequently dichloromethane/methanol 30:1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07202243B2 |
| Quelldatensatz | uspto-grants-2007_04 |
| ORD ID | ord-32ae0f887b1a4abbbf38df4bcbecd908 |
| Quellennotiz | uspto-grants-2007_04 |