Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 2,6-Dimethylbenzyl Chloride | HCID 221154 | — |
| Edukt | Potassium | HCID 5462222 | — |
| Edukt | 5-Methyl-2-nitropyridin-3-ol | HCID 21766019 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | HCID 21717332 | HCID 21717332 | 81,1% |
Reaktionsschritte
To 0.52 g (8.02 mmol) of 87% KOH and 0.15 g q-iodide in 6 ml 95% ethanol was added a solution of 3-hydroxy-5-methyl-2-nitropyridine (1.2 g, 7.79 mmol) in 25 ml of ethanol. To the resulting suspension of the potassium salt was added dropwise a solution of 2,6-dimethyl benzylchloride (1.24 g, 8.02 mmol) in 13 ml of ethanol. The reaction mixture was refluxed for 1 h. More 87% KOH (0.16 g) and 2,6-dimethylbenzylchloride (0.38 g) were added. The reaction mixture was refluxed for additional 70 min. The mixture was filtered and the inorganic salts were washed with ethanol and methylene chloride. The organic layer was evaporated in vacuo. The residue was dissolved in methylene chloride, washed with aqueous NaHCO3, dried and evaporated in vacuo. The residue was suspended in ether/isopropanol and filtered to give 1.72 g (81%) of the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US06265415B1 |
|---|
| Quelldatensatz | uspto-grants-2001_07 |
|---|
| ORD ID | ord-75f2cc39dc7a474190888369be86b8ef |
|---|
| Quellennotiz | uspto-grants-2001_07 |
|---|