HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triphenylphosphine → methyl (E)-3-(2-{3-[6-oxo-3-(3,4,5-trifluorophenyl)-6H-pyridazin-1-ylmethyl]phenyl}pyrimidin-5-yl)acrylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Edukt | methyl (E)-3-[2-(3-hydroxymethylphenyl)pyrimidin-5-yl]acrylate | HCID 58289762 | — |
| Edukt | 6-(3,4,5-trifluorophenyl)-2H-pyridazin-3-one | HCID 59406809 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | methyl (E)-3-(2-{3-[6-oxo-3-(3,4,5-trifluorophenyl)-6H-pyridazin-1-ylmethyl]phenyl}pyrimidin-5-yl)acrylate | HCID 59484916 | — |
Reaktionsschritte
47.2 90 mg (0.4 mmol) of 6-(3,4,5-trifluorophenyl)-2H-pyridazin-3-one and 111 mg (0.41 mmol) of methyl (E)-3-[2-(3-hydroxymethylphenyl)-pyrimidin-5-yl]acrylate are suspended in 3 ml of THF with 200 mg (0.6 mmol) of polymer-bound triphenylphosphine (about 3 mmol of triphenylphosphine per g), and the mixture is shaken at room temperature for 30 min. The mixture is cooled to 0° C., and 95 μl (0.6 mmol) of diethyl azodicarboxylate are added. The reaction mixture is shaken at room temperature for 24 h. The reaction mixture is purified by means of preparative
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09284300B2 |
| Quelldatensatz | uspto-grants-2016_03 |
| ORD ID | ord-4176126a18b64e559d4311e2615b11c3 |
| Quellennotiz | uspto-grants-2016_03 |