関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2,3,5-Trimethyl-1-oxidopyridin-1-ium | HCID 10486907 | — |
| 生成物 | 4-Nitro-2,3,5-trimethylpyridine, 1-oxide | HCID 11217611 | 93.1% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425634B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-e3543f00d349451ab8e265392c8c426b |
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| 出典メモ | uspto-grants-2008_09 |
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