참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitric Acid | HCID 944 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 2,3,5-Trimethyl-1-oxidopyridin-1-ium | HCID 10486907 | — |
| 생성물 | 4-Nitro-2,3,5-trimethylpyridine, 1-oxide | HCID 11217611 | 93.1% |
반응 단계
The 2,3,5-trimethylpyridine1-oxide (11.0 g, 80.2 mmol) obtained in the step (11b) was mixed with sulfuric acid (34.1 g, 348 mmol). After fuming nitric acid (5.50 ml, 133 mmol) was added dropwise to this mixture at room temperature, the mixture was stirred at 80° C. for 9 hours. The reaction mixture was cooled to room temperature and thereafter poured into ice. The obtained aqueous solution was extracted with chloroform three times. Organic layers were combined and dried over anhydrous magnesium sulfate, filtered and concentrated to obtain the title compound (13.6 g, yield: 93.1%) as a yellow 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-e3543f00d349451ab8e265392c8c426b |
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| 출처 메모 | uspto-grants-2008_09 |
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