HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
m-Chloroperbenzoic acid → 2-Chloro-4-methylpyridine 1-oxide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | m-Chloroperbenzoic acid | HCID 70297 | — |
| Edukt | 2-Chloro-4-methylpyridine | HCID 77248 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | 2-Chloro-4-methylpyridine 1-oxide | HCID 12487484 | 464,3% |
Reaktionsschritte
40% meta-chloroperbenzoic acid (13.5 g, 31.4 mmol) was added at ambient temperature to a solution of 2-chloro-4-methyl-pyridine (2.0 g, 1.5 mmol) in chloroform (20 mL) and heated at reflux for 24 h. After allowing to cool, the mixture was washed with water followed by sodium bicarbonate solution. The separated organic phase was further washed with water and brine, dried over anhydrous sodium sulfate and concentrated to give a residue which was purified by column chromatography over silica gel (60-120 mesh) using 10% methanol in ethyl acetate as eluent to afford 2-chloro-4-methyl-pyridine 1-oxide (1.0 g, 45%) as a deep brown oily liquid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08524705B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-c2ddec53bd744cd7b5a933c42f3d5d64 |
| Quellennotiz | uspto-grants-2013_09 |