HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Phosphorus oxychloride → 2,6-Dichloro-4-methylpyridine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 2-Chloro-4-methylpyridine 1-oxide | HCID 12487484 | — |
| Produkt | 2,6-Dichloro-4-methylpyridine | HCID 10898997 | 43% |
Reaktionsschritte
A mixture of 2-chloro-4-methyl-pyridine 1-oxide (1.0 g, 7.0 mmol) and phosphorus oxychloride (10 mL) was heated at reflux for 4 h. The volatiles were evaporated and the residue dissolved in ethyl acetate. The solution was washed with ice-water followed by sodium bicarbonate solution. The organic phase was again washed with water, brine solution, dried over anhydrous sodium sulfate and concentrated to obtain a residue which was purified by column chromatography over silica gel (60-120 mesh) using petroleum ether as eluent to afford 2,6-dichloro-4-methyl-pyridine (491 mg, 43%) as a white solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08524705B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-51cb4aae7be0496d84ff01fb90662113 |
| Quellennotiz | uspto-grants-2013_09 |