참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Piperidine, 1-(2-chloroethyl)-, hydrochloride | HCID 74826 | — |
| 반응물 | 3-Pyridinecarboxamidine | HCID 202043 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | O-(2-piperidinoethyl)-3-pyridinehydroximoyl chloride hydrochloride | HCID 86754158 | 23.5% |
반응 단계
After dissolving 6.45 g (47.0 mmoles) of 3-pyridinecarboxamidine in 120.4 ml of 0.83N potassium hydroxide solution in ethanol under stirring, 8.65 g (47.0 mmoles) of 1-(2-chloroethyl)piperidine hydrochloride are added under stirring, then the reaction mixture is boiled under reflux for 4 hours. The precipitated potassium chloride is filtered off, the filtrate is clarified by activated carbon and evaporated. The residue is dissolved in 100 ml of chloroform, and the organic solution is washed 3 times with 100 ml of 1N sodium hydroxide solution each, then with 50 ml of water. The organic phase is dried over sodium sulfate and evaporated. The residue is purified by column chromatography (adsorbent: recrystallized from ether to give 2.69 g (23.5%) of the aimed product, m. p.: 81-83° C. (from ether).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05919796 |
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| 출처 데이터셋 | uspto-grants-1999_07 |
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| ORD ID | ord-2c1413ce3f0b41d98b12e6d072763aa8 |
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| 출처 메모 | uspto-grants-1999_07 |
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