関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Hydrogen iodide | HCID 24841 | — |
| 反応物 | 6-Chloronicotinic acid | HCID 79222 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 6-Iodopyridine-3-carboxylic acid | HCID 819062 | — |
反応手順
To 27.97 g (186.6 mmol) of sodium iodide cooled to -78° C. was added 121.77 g (71.6 ml, 952.0 mmol) of hydriodic acid (57 wt %). The reaction mixture was allowed to warm slightly with stirring for 5 minutes, and then 30.00 g (190.4 mmol) of 6-chloronicotinic acid was added. The resulting mixture was allowed to warm to room temperature with stirring and then heated at 120°-125° C. in an oil bath for 42 hours. A dark brown layer formed above the yellow solid material. The reaction mixture was allowed to cool to room temperature and then poured into acetone (chilled to 0° C.). The resultant yellow solid was collected by filtration, washed with 200 ml of 1N NaHSO3 solution, and dried in high vacuum (3 mm Hg) to give the title compound as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05618931 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-b6665b274db740d495d2125d751f579c |
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| 出典メモ | uspto-grants-1997_04 |
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