関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Potassium bisulfate | HCID 516920 | — |
| 反応物 | HCID 178490904 | HCID 178490904 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178490906 | HCID 178490906 | 94% |
反応手順
Diiodine (0.547 g, 2.16 mmol) in ethanol (5 mL) was added dropwise over 5 minutes to a solution of 1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-4-ol (0.50 g, 1.96 mmol, prepared similarly as that described in WO 2007/103308) in absolute ethanol (20 mL) at 0° C. The reaction was stirred at 0° C. for 3 hours, followed by addition of 5% sodium bicarbonate (20 mL). The mixture was concentrated to give a slurry. The pH was then adjusted with saturated KHSO4 to a pH of 4. The resulting solid was collected by filtration and dried to give 5-iodo-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-4-ol (0.70 g, 94%). MS APCI (+) m/z 382.0 detected.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08372842B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-526f04bf4ae94df5a13eaf4fe84dee0b |
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| 出典メモ | uspto-grants-2013_02 |
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