HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → (2-Aminopyridin-3-yl)methanol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 2-Aminonicotinic acid | HCID 72930 | — |
| Edukt | Sodium | HCID 5360545 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | (2-Aminopyridin-3-yl)methanol | HCID 11159325 | — |
Reaktionsschritte
Lithium aluminum hydride (12.4 g, 326.7 mmol) was portionwisely added to a suspension of 2-amino-3-carboxypyridine (30.0 g, 217.2 mmol) in THF (350 mL) at 0° C. Once the addition was completed, the reaction mixture was stirred at room temperature for 15 minutes and then at reflux overnight. The mixture was then cooled to 0° C. and hydrolyzed by the successive addition of water (18 mL), a solution of sodium hydroxyde (18 mL) and water (30 mL) again. The resulting white suspension was filtered on Clarcel® and the cake was washed with THF (200 mL) and a mixture of CHCl3/MeOH (250 mL, 9:1). After concentration to dryness of the filtrate, the title product was obtained as a yellow solid (24.2 g, 90%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08846711B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-212e7e6947c5488984cdbd83e5ff1afa |
| Quellennotiz | uspto-grants-2014_09 |