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Hydrochloric Acid → 6-Methoxy-4-methylpyridin-3-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Methoxy-4-methyl-5-nitropyridine | HCID 243169 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 6-Methoxy-4-methylpyridin-3-amine | HCID 243170 | 93.1% |
反応手順
A mixture of stannous chloride dihydrate (41 g) and concentrated hydrochloric acid (40 ml) was added slowly to a solution of 2-methoxy-4-methyl-5-nitropyridine (5.1 g) in acetic acid (40 ml), maintaining the temperature below 35° C. The resulting mixture was stirred at room temperature for 2 hours, and then allowed to stand overnight in the refrigerator. The solid was collected and both solid and supernatant were separately basified with a 20% sodium hydroxide solution. The product was extracted with chloroform, combined, dried (anhydrous magnesium sulfate) and concentrated to give 3.9 g of the title compound as a solid, suitable for use in the next reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05620974 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-da1bc058a21e4a1093907d85c422255a |
| 出典メモ | uspto-grants-1997_04 |