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Nitric Acid → 4-Nitrothiophene-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 2-Thiophenecarboxylic acid | HCID 10700 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | 4-Nitrothiophene-2-carboxylic acid | HCID 268680 | — |
反応手順
2-Thiophenecarboxylic acid (6.4 g, 50 mM) was suspended in acetic anhydride (15 ml) and fuming nitric acid (16 ml) in glacial acetic acid (25 ml) added slowly over 1 hour with stirring, while keeping the temperature of the reaction mixture below 30° C. The reaction mixture was stirred at ambient temperature for 2 hours. The product was purified by subjecting to chromatography (470 ml) on HP20SS resin using methanol/(water+1% acetic acid): 0/100→50/50 as eluant. The pure title compound was obtained (1.3 g) together with a mixture of 4- and 5- nitrothiophene-2-carboxylic acid (4.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05519015 |
| 出典データセット | uspto-grants-1996_05 |
| ORD ID | ord-6eb7bb3d44df48c598ace63eb0f97df3 |
| 出典メモ | uspto-grants-1996_05 |