HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methylhydrazine → 1-Methyl-3-phenyl-1H-pyrazol-5-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methylhydrazine | HCID 6061 | — |
| Edukt | Benzoylacetonitrile | HCID 64799 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 1-Methyl-3-phenyl-1H-pyrazol-5-amine | HCID 517779 | 71,2% |
Reaktionsschritte
A mixture of benzoyl acetonitrile (2.0 g, 13.778 mmol) and methyl hydrazine (0.698, 15.156 mmol) in methanol (10 mL) was irradiated under microwave conditions at 110° C. for 90 min. The reaction mixture was cooled to rt and poured into rapidly stirred ice cold water. The obtained solid was collected by filtration, dried under vacuum and triturated with a mixture of pentane-hexane (˜10 mL) to yield a white solid (1.7 g, 71%). [1H-NMR (CDCl3, 300 MHz) δ 7.82-7.65 (m, 2H), 7.45-7.20 (m, 3H), 5.90 (s, 1H), 3.75 (s, 3H), 3.55 (s, 2H); LCMS RtA=0.824 min; [M+H]+=174.1]
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08742106B2 |
| Quelldatensatz | uspto-grants-2014_06 |
| ORD ID | ord-13a444bbc6634ce09bcbd8cf08acef13 |
| Quellennotiz | uspto-grants-2014_06 |