関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 6-Methylpyridine-2-carboxylic acid | HCID 70282 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 6-methylpyridine-2-carboxylate | HCID 73022 | — |
反応手順
To a suspension of 6-methyl-pyridine-2-carboxylic acid (10 g, 72.9 mmol) in methylene chloride (200 mL) cooled to 0° C. is added methanol (10 mL), 4-dimethylaminopyridine (11.6 g, 94.8 mmol), and EDC (18.2 g, 94.8 mmol). The mixture is stirred at room temperature for 6 h, washed with water and brine, and dried over sodium sulfate. The mixture is filtered and concentrated in vacuo. The residue is chromatographed on SiO2 (50% ethyl acetate/hexanes) to yield the title compound, 9.66 g (92%), as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07087626B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-6f91fd8aa044449a8fb53ad9db2adc17 |
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| 出典メモ | uspto-grants-2006_08 |
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