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Hydroxyamine hydrochloride → 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carbonitrile | HCID 59570359 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carboxamide | HCID 86647339 | 102.2% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08318776B2 |
| 出典データセット | uspto-grants-2012_11 |
| ORD ID | ord-17346a5123b34d9aa66625967188cc8a |
| 出典メモ | uspto-grants-2012_11 |