関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,6-Dichloro-3-methylpyridine | HCID 817088 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 2,6-Dichloro-3-methyl-5-nitropyridine | HCID 12265428 | 86% |
反応手順
A mixture of 2,6-dichloro-3-methylpyridine (2.20 g, 13.6 mmol) in concentrated sulfuric acid (11.3 mL) was treated with fuming nitric acid (6.65 mL) and heated to 110° C. for 3 hours. The reaction mixture was poured into ice-water and neutralized with 2N sodium hydroxide. The mixture was extracted with dichloromethane (3×70 mL) and the combined extracts were dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to yield 2,6-dichloro-3-methyl-5-nitropyridine (2.43 g, 86%). 400 M Hz 1H NMR (DMSO-d6) δ: 8.66 (s, 1H), 2.39 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08501770B2 |
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| 出典データセット | uspto-grants-2013_08 |
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| ORD ID | ord-cd1dcc60bc014ac09efbaf37aebd3954 |
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| 出典メモ | uspto-grants-2013_08 |
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