참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Ethyl-2-methylpyridine | HCID 34087 | — |
| 반응물 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Ethyl-2-methylpyridine1-oxide | HCID 59792526 | 89.6% |
반응 단계
First, 3-ethyl-2-methylpyridine (7.25 g, 59.8 mmol) was dissolved in dichloromethane (dehydrated)(100 ml) and 3-chloroperbenzoic acid (19.0 g, 71.6 mmol, as the content was regarded as 65%) was added in a nitrogen atmosphere at ice-cooling temperature. The mixture was stirred at room temperature for 90 hours. To the reaction mixture, a saturated aqueous sodium hydrogen carbonate solution was added. The aqueous layer was extracted twice with dichloromethane and three times with chloroform. The organic layers were combined, dried over anhydrous magnesium sulfate, filtrated and concentrated. The residue was purified by silica gel column chromatography (silica gel: 100 g, elution solvent: heptane, ethyl acetate/methanol=10/1) to obtain the title compound (7.35 g, yield: 89.6%) as a reddish solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07425634B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-8aabbf1aa12a4bc8be4bfd05ef2cb690 |
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| 출처 메모 | uspto-grants-2008_09 |
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