化工社化工社 化学情報印刷レポート · 研究参考用
Lithium Hydroxide → 3-Nitropyridine-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | Ethyl 3-nitropyridine-2-carboxylate | HCID 18376573 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Nitropyridine-2-carboxylic acid | HCID 18376612 | 95.2% |
反応手順
To a solution of 2-ethoxycarbonyl-3-nitropyridine (0.5 g, 2.5 mmol, 1 eq.) in 20 mL of methanol and 5 mL of water was added lithium hydroxide (0.2 g, 4.5 mmol, 1.8 eq.) and the mixture stirred for 16 hours at ambient temperature. The reaction was concentrated and 50 mL of 1 N KOH was were added. The solution was washed with 25 mL of ethyl actetate, acidified with 1 N HCl, and extracted with ethyl acetate (3×50 mL). The combined ethyl acetate extractions were dried over sodium sulfate and concentrated to give 2-carboxy-3-nitropyridine as a yellow solid (0.4 g, 95% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06380221B1 |
| 出典データセット | uspto-grants-2002_04 |
| ORD ID | ord-096478117006417c96428ac8a4cffbb4 |
| 出典メモ | uspto-grants-2002_04 |