참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl 3-oxo-3-(pyridin-2-yl)propanoate | HCID 2736461 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178472895 | HCID 178472895 | 61.5% |
반응 단계
To a stirred solution of ethyl picolinoylacetate (0.500 g, 2.6 mmol) in acetic acid (0.5 mL) was added a solution of sodium nitrite (0.238 g, 3.4 mmol) in water (0.5 mL), dropwise. The resulting solution was stirred at room temperature for 2 hours after which water (0.5 mL) was added and the reaction was stirred for a further 2 hours. The mixture was extracted with Et2O and the combined organic phase was washed with water, saturated sodium bicarbonate solution and brine, dried over MgSO4 and the solvent removed in vacuo to afford ethyl 2-(hydroxyimino)-3-oxo-3-(pyridin-2-yl)propanoate (0.353 g, 1.6 mmol, 61%) as a white solid. 1H NMR (DMSO) δ 1.17 (3H, t), 4.22 (2H, q), 7.74 (1H, m), 8.04-8.11 (2H, m), 8.74 (1H, m), 12.87 (1H, s). LCMS (2) Rt: 1.09 min; m/z (ES+) 223.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09187465B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-4540f02f705b4cc6b8531fc74e77a5ee |
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| 출처 메모 | uspto-grants-2015_11 |
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