참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 반응물 | 1-(Dimethylamino)-4-piperidinone | HCID 56737782 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 1-Dimethylamino-piperidin-4-one oxime | HCID 86671304 | 68.3% |
반응 단계
19.2 g 1-Dimethylamino-piperidin-4-one (prepared as described in Journal of Medicinal & Pharmaceutical Chemistry, 4, 423-36; 1961) and 30 g triethylamine are dissolved in 80 ml methanol. 18.8 g hydroxylamin hydrochloride is added in portions at ambient temperature. The internal temperature raises during the addition to 37° C. Then the mixture is heated to reflux for 3 hours, allowed to cool to room temperature, and then the solvent evaporated. The residue is partitioned between ethyl acetate and aqueous sodium bicarbonate. The organic layer is dried over sodium sulfate, and the solvent evaporated. Thus, 14.5 g 1-Dimethylamino-piperidin-4-one oxime is obtained. 1H-NMR (CDCl3): 8.10 ppm (s, broad, 1H), 2.75 ppm (m, 6H), 2.40 ppm (m, 2H), 2.40 ppm (s, 6H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08703165B2 |
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| 출처 데이터셋 | uspto-grants-2014_04 |
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| ORD ID | ord-26a3a45656db442682014dd6ec817748 |
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| 출처 메모 | uspto-grants-2014_04 |
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