HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydroxyamine hydrochloride → 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carboxamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydroxyamine hydrochloride | HCID 443297 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carbonitrile | HCID 59570359 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carboxamide | HCID 86647339 | 102,2% |
Reaktionsschritte
To 7 ml of ethanol were added 0.44 g of sodium bicarbonate and 0.37 g of hydroxylamine hydrochloride, and the mixture was heated to reflux for 1 hour. After allowing to cool, 0.7 g of 4-(2,2,2-trifluoro-1-methyl-ethyl)pyridine-2-carbonitrile was added at 0° C., and the mixture was stirred for 4 hours, and concentrated. To the residue was added water, the resultant solution was extracted with ethyl acetate three times, and the organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.78 g of 4-(2,2,2-trifluoro-1-methyl-ethyl)pyridine-2-carboxamide=oxime.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08318776B2 |
| Quelldatensatz | uspto-grants-2012_11 |
| ORD ID | ord-17346a5123b34d9aa66625967188cc8a |
| Quellennotiz | uspto-grants-2012_11 |