関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-Methylpyridine-2-carbonitrile | HCID 819928 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Methylpyridine-2-carboxamide | HCID 16641023 | 97% |
反応手順
A mixture of 3-methylpicolinonitrile (2.36 g, 20 mmol) and conc. sulfuric acid (12.5 mL) was stirred at 80° C. for 25 min. The solution was cooled to rt, poured into water (80 mL), followed by addition of sat. Na2CO3 (aq.) until pH ˜7. The resulting mixture was extracted with DCM (3×) and the combined organic layer was dried over MgSO4 and concentrated in vacuo to provide 3-methylpicolinamide as a white solid (2.65 g, 97%). 1H NMR (CDCl3, 400 MHz) δ 8.43 (dd, 1H), 7.93 (brs, 1H), 7.62 (dd, 1H), 7.35 (dd, 1H), 5.44 (brs, 1H), 2.76 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09440982B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-af1e112a241f4df6851c8639a4e9428b |
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| 出典メモ | uspto-grants-2016_09 |
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