참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,1-Dimethyl-4-oxopiperidin-1-ium iodide | HCID 11149497 | — |
| 반응물 | 2-(Pyrimidin-5-yl)propan-2-amine | HCID 45080140 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 1-(2-(5-Pyrimidinyl)-prop-2-yl)-4-oxopiperidine | HCID 21471595 | 34.1% |
반응 단계
To a stirred mixture of 2-(5-pyrimidinyl)-2-propylamine (660 mg), ethanol (9 mL) and K2CO3 (665 mg) heated to reflux was added dropwise over 30 min, a solution of 1,1-dimethyl-4-oxopiperidinium iodide (1.9 g) in water (36 mL). When the addition was complete, the mixture was heated under reflux for an additional 2 h, cooled, basified to pH 10 with Na2CO3 and extracted with ethyl acetate (3 .Yen.100 mL). The combined organic extracts were dried over MgSO4 and concentrated under reduced pressure. Column chromatography over silica gel, eluting with a methylene chloride; 5% methanol gave 360 mg of 1-(2-(5-pyrimidinyl)-prop-2-yl)-4-oxopiperidine as an oil: 1H NMR (400 MHz, CDCl3) 9.13 (s, 1H), 8.95 (s, 2H), 2.79 (t, 4H), 2.44 (t, 4H), 1.47 (s, 6H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05691323 |
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| 출처 데이터셋 | uspto-grants-1997_11 |
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| ORD ID | ord-2be575fc1c034a92b43d4da955ac96e3 |
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| 출처 메모 | uspto-grants-1997_11 |
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