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Ethanol → N-[(2R,6S)-2,6-Dimethylcyclohexylidene]hydroxylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 2,6-Dimethylcyclohexanone | HCID 17780 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | N-[(2R,6S)-2,6-Dimethylcyclohexylidene]hydroxylamine | HCID 21723229 | — |
| 生成物 | trans-2,6-Dimethylcyclohexanone oxime | HCID 40531046 | — |
反応手順
5 g of 2,6-dimethylcyclohexanone and 5.51 g of hydroxylamine hydrochloride were suspended to 80 ml of ethanol, then 9.4 g of pyridine was dropped at 0° C. The mixture was stirred at room temperature for 4 hours, then the reaction mixture was concentrated. Water was added to the residue and extracted with ethyl acetate three times. The organic layers were joined, washed with saturated aqueous solution of sodium chloride, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 3.1 g of cis-2,6-dimethylcyclohexanoneoxime and 1.3 g of trans-2,6-dimethylcyclohexanoneoxime.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08101753B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-632e3ea77dfc479bbd2fd58a8a6cd439 |
| 出典メモ | uspto-grants-2012_01 |