Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydroxyamine hydrochloride → 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carbonitrile | HCID 59570359 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 4-(2,2,2-Trifluoro-1-methyl-ethyl)pyridine-2-carboxamide | HCID 86647339 | 102.2% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08318776B2 |
| 출처 데이터셋 | uspto-grants-2012_11 |
| ORD ID | ord-17346a5123b34d9aa66625967188cc8a |
| 출처 메모 | uspto-grants-2012_11 |