HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Cesium carbonate → 3-(2-Fluoro-4-nitrophenoxy)-2,6-dimethyl-pyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 2,6-Dimethyl-3-pyridinol | HCID 70732 | — |
| Edukt | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 3-(2-Fluoro-4-nitrophenoxy)-2,6-dimethyl-pyridine | HCID 59287319 | 92,1% |
Reaktionsschritte
To a room temperature solution of 2,6-dimethyl-3-pyridinol (3 g, 24.35 mmol) in THF (30 ml) was added cesium carbonate (15.87 g, 48.71 mmol) and 3,4-difluoro-1-nitro-benzene (3.87 g, 24.35 mmol). The reaction mixture was heated at reflux for 2 hours. After cooling to room temperature the solids were filtered off and the filtrate was evaporated till dryness. The crude product was purified by column chromatography (silica gel; DCM to DCM/MeOH(NH3) up to 2% as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 9 (5.88 g, 92%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09067891B2 |
| Quelldatensatz | uspto-grants-2015_06 |
| ORD ID | ord-6b03cd9d70f24a349c02bb89551cb28b |
| Quellennotiz | uspto-grants-2015_06 |