HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl iodide → 1-Methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | 2-Hydroxynicotinic acid | HCID 69114 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-Methyl-2-oxo-1,2-dihydropyridine-3-carboxylic acid | HCID 1201510 | — |
Reaktionsschritte
To 2-oxo-1H-pyridine-3-carboxylic acid (2.00 g, 14.4 mmol) in methanol (20 mL) was added a solution of KOH (1.60 g, 28.5 mmol) in water (3 mL) and the mixture was vigorously stirred until a thick suspension formed. Iodomethane (10 μL, 0.16 mmol) was added and the mixture was heated at reflux for 1.5 h. The mixture was concentrated to ⅓ volume and was acidified to pH 1 with 6N HCl. The solids were filtered off and were washed with water (3×2 mL) and acetonitrile (2×2 mL), and then dried in vacuo to give 1-methyl-2-oxo-pyridine-3-carboxylic acid as a white solid. ESI-MS m/z calc 153.0. found 154.1 (M−1)−. Retention time: 0.65 minutes (3 min run).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08598164B2 |
| Quelldatensatz | uspto-grants-2013_12 |
| ORD ID | ord-03398f8c8f004d69ba67d611336215a2 |
| Quellennotiz | uspto-grants-2013_12 |