化工社化工社 化学情報印刷レポート · 研究参考用
Iodine → 5-iodo-N-methoxy-N-methyl-1H-indazole-3-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Bistrifluoroacetoxyiodobenzene | HCID 12041285 | — |
| 反応物 | N-Methoxy-N-methyl-1H-indazole-3-carboxamide | HCID 16036867 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-iodo-N-methoxy-N-methyl-1H-indazole-3-carboxamide | HCID 20580738 | 72% |
反応手順
To a solution of N-methoxy-N-methyl-1H-indazole-3-carboxamide (12.4 g, 60.42 mmol) in CH2Cl2 (200 mL) was added bis(trifluoroacetoxy)iodobenzene (28.78 g, 66.74 mmol), followed by dropwise addition of iodine (9.22 g, 36.33 mmol) in CH2Cl2 at rt. The reaction was stirred overnight, after which 300 mL saturated NaHSO3 was added and a solid began to precipitate, which was then filtered. The filtrate was concentrated and triturated with a small amount of CH2Cl2. The combined solids were dried to give 5-iodo-N-methoxy-N-methyl-1H-indazole-3-carboxamide (14.4 g, 72%) as a yellow solid.
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-bf0c526919e04f2bb8dbe14fc2f2e7db |
| 出典メモ | uspto-grants-2012_06 |