関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 6-Fluoropyridin-3-ol | HCID 2763108 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Fluoro-2-iodopyridin-3-ol | HCID 19597673 | 19% |
反応手順
6-Fluoro-3-hydroxypyridine (870 mg) and iodine (9.76 g) were dissolved in a mixed solvent composed of methanol (20 ml) and water (10 ml) to prepare a solution which was then stirred at room temperature for 120 hr. Thereafter, sodium sulfite was added until the solution became transparent. Methanol in the reaction solution was removed under the reduced pressure, water was added to the residue, and the mixture was extracted with chloroform. The chloroform layer was washed with water and saturated brine and was dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using acetone-chloroform to give 6-fluoro-2-iodo-pyridin-3-ol (350 mg, yield 19%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560558B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-84827c35812b42ff930dd8d9445a6fbb |
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| 出典メモ | uspto-grants-2009_07 |
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