関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-(Methylthio)aniline | HCID 66038 | — |
| 反応物 | 2-Fluoroisonicotinic acid | HCID 345360 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-[[4-(Methylthio)phenyl]amino]isonicotinic acid | HCID 28400355 | — |
反応手順
To a solution of 2-fluoroisonicotinic acid (620 mg, 4.95 mmol) and 4-(methylthio)aniline (0.984 mL, 8.42 mmol) in N,N-dimethylformamide (20 mL) was added sodium hydride (792 mg, 19.8 mmol), and the resulting mixture was stirred under an argon atmosphere at 85° C. for 5 hr. After cooling, acetic acid (1.2 mL) was added to the reaction mixture, and the mixture was concentrated under reduced pressure. Ethyl acetate and water were added to the residue, the mixture was stirred for 20 min, and the precipitate was collected by filtration to give crude 2-[[4-(methylthio)phenyl]amino]isonicotinic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08492378B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-421b9b0c69434c2cabddaf72f72d3971 |
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| 出典メモ | uspto-grants-2013_07 |
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