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Iodine → HCID 178519380、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1H-Indazole-5-carboxaldehyde | HCID 21250644 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | HCID 178519380 | HCID 178519380 | 64.5% |
反応手順
To a solution of 1H-indazole-5-carboxaldehyde (3.75 g, 25.7 mmol) in dioxane (120 mL) was added a solution of NaOH (15.48 g, 384.9 mmol) in water (120 mL). To this solution, iodine (8.2 g, 32 mmol) was added. After 1 hr at rt, more iodine (8.2 g, 32 mmol) was added, and the reaction mixture was stirred for an additional 1 hr at rt. After removal of most of the dioxane in vacuo, the reaction mixture was extracted with EtOAc, washed with brine, dried, and concentrated. The crude product was purified by flash chromatography to afford 3-iodo-1H-indazole-5-carboxaldehyde (4.5 g, 64.5%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198456B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-95be1ffb397d42808583323e2778abd2 |
| 出典メモ | uspto-grants-2012_06 |