関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethylsilyldiazomethane | HCID 167693 | — |
| 反応物 | 4-Iodo-2-methoxypyridine-3-carboxylic acid | HCID 18439940 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 4-iodo-2-methoxynicotinate | HCID 58819970 | — |
反応手順
4-Iodo-2-methoxynicotinic acid (800 mg, 2.87 mmol) is dissolved in MeOH (7 mL) and cooled at 0° C. Trimethylsilyldiazomethane (9 mL, 2M in hexane, 4.5 mmol) is added slowly over 20 minutes. The reaction mixture is brought to room temperature and stirred for 16 hours. The reaction mixture is concentrated and purified by silica gel column chromatography using hexane:ethyl acetate as eluent to afford the desired compound. 1H NMR 400 MHz (DMSO-d6) δ 7.88 (d, 1H, J=5.6 Hz), 7.34 (d, 1H, J=5.6 Hz), 4.12 (s, 3H), 3.84 (s, 1H); MS m/z 294.1 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08546370B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-38bdaf2c97254d0e88dda5193b8834be |
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| 出典メモ | uspto-grants-2013_10 |
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