HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium Hydroxide → 3-Nitropyridine-2-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | Ethyl 3-nitropyridine-2-carboxylate | HCID 18376573 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 3-Nitropyridine-2-carboxylic acid | HCID 18376612 | 95,2% |
Reaktionsschritte
To a solution of 2-ethoxycarbonyl-3-nitropyridine (0.5 g, 2.5 mmol, 1 eq.) in 20 mL of methanol and 5 mL of water was added lithium hydroxide (0.2 g, 4.5 mmol, 1.8 eq.) and the mixture stirred for 16 hours at ambient temperature. The reaction was concentrated and 50 mL of 1 N KOH was were added. The solution was washed with 25 mL of ethyl actetate, acidified with 1 N HCl, and extracted with ethyl acetate (3×50 mL). The combined ethyl acetate extractions were dried over sodium sulfate and concentrated to give 2-carboxy-3-nitropyridine as a yellow solid (0.4 g, 95% yield).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06380221B1 |
| Quelldatensatz | uspto-grants-2002_04 |
| ORD ID | ord-096478117006417c96428ac8a4cffbb4 |
| Quellennotiz | uspto-grants-2002_04 |