HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → Raf265
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 4-(Trifluoromethyl)phenyl isothiocyanate | HCID 137134 | — |
| Edukt | 2-Chloro-1-methylpyridinium iodide | HCID 167069 | — |
| Edukt | 1,2-Benzenediamine,n1-methyl-4-[[2-[5-(trifluoromethyl)-1h-imidazol-2-yl]-4-pyridinyl]oxy]- | HCID 57531890 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Acetonitrile | HCID 6342 | — |
| Produkt | Raf265 | HCID 11656518 | 61,1% |
Reaktionsschritte
4-Trifluoromethylphenyl isothiocyanate (200 mg, 1 mmol) was added to a mixture of 4-(2-(5-(trifluoromethyl)-1H-imidazol-2-yl)pyridin-4-yloxy)-N1-methylbenzene-1,2-diamine (350 mg, 1 mmol) in 3 mL of acetonitrile. After stirring for 20 min at ambient temperature, HPLC analysis showed complete conversion. Triethylamine (0.3 mL, 2.2 mmol) was added followed by 2-chloro-1-methylpyridinium iodide (270 mg, 1.05 mmol). The reaction mixture was heated to 50° C. for 5 h. The heating was stopped and 1.5 mL of water was added. After stirring the mixture for 2 h, the solid was collected by filtration and washed with 2:1 acetonitrile/water (3×1 mL) to afford 317 mg (61%) of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07732465B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-41569efb36284549a33e200ea2966f74 |
| Quellennotiz | uspto-grants-2010_06 |