関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 反応物 | HCID 71093647 | HCID 71093647 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-(4-iodo-1-methyl-1H-pyrazol-5-yl)-5-(trifluoromethyl)pyridine | HCID 71093632 | — |
反応手順
N-Iodosuccinimide (95%, 427 mg, 1.80 mmol) was added to a mixture of 2-(1-methyl-1H-pyrazol-5-yl)-5-(trifluoromethyl)pyridine (C13) (390 mg, 1.72 mmol) and acetic acid (4 mL), and the reaction mixture was heated at 70° C. for 1 hour. The mixture was concentrated in vacuo and subjected to silica gel chromatography (Gradient: 0% to 100% ethyl acetate in heptane) to afford the product as a white solid. Yield: 524 mg, 1.48 mmol, 86%. APCI m/z 353.8 (M+1). 1H NMR (400 MHz, CD3OD) δ 3.89 (s, 3H), 7.66 (s, 1H), 8.00 (br d, J=8 Hz, 1H), 8.17 (br dd, J=8, 2 Hz, 1H), 8.83 (br d, J=2 Hz, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08829010B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-5f73ead2fb124b9bbaf38bf01016478a |
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| 出典メモ | uspto-grants-2014_09 |
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