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Hydrochloric Acid → Methyl 2-acetamidoisonicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 2-Acetamidopyridine-4-carboxylic acid | HCID 3774466 | — |
| 生成物 | Methyl 2-acetamidoisonicotinate | HCID 22185175 | 84% |
反応手順
To 2-(acetamido)pyridine-4-carboxylic acid (25 g, 139 mmol) was added a saturated solution of anhydrous hydrogen chloride in methanol (600 mL). The cloudy suspension was stirred for 16 h at RT and refluxed for 24 h. The resulting solution was concentrated, dissolved in chloroform, washed with saturated sodium bicarbonate, brine, dried (magnesium sulfate) and concentrated to give the title compound as a white solid (17.86 g, 84%). TLC Rf 0.55 (5% methanol/chloroform); 1H NMR (CDCl3) δ3.96 (3H, s), 4.80 (2H, s),7.12 (1H, J=5 Hz, d), 7.19 (1H, s), 8.10 (1H, d, J=5 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06403578B1 |
| 出典データセット | uspto-grants-2002_06 |
| ORD ID | ord-ac748b9e140541a98c86945c2dde49df |
| 出典メモ | uspto-grants-2002_06 |