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Iodine → HCID 178506566、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 | 1H-Indazole | HCID 9221 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178506566 | HCID 178506566 | 99.4% |
反応手順
In a 50 mL round-bottomed flask, indazole (0.80 g, 6.8 mmol) was dissolved in DMF (14 mL). Iodine (3.4 g, 13.5 mmol) was added followed by potassium hydroxide (1.47 g, 26.2 mmol). The dark reaction mixture was stirred at room temperature for 1.25 h then was quenched with 10% aq NaHSO3 and extracted with diethyl ether (2×). The combined organic layers were washed with water and brine then dried over sodium sulfate, filtered and concentrated to give 1.65 g (95%) of 3-iodo-1H-indazole as a light yellow solid. 1H NMR (CDCl3, 300 MHz): δ (ppm) 10.56 (br. s, 1H), 7.47-7.57 (m, 3H), 7.23-7.30 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658646B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-95d34199a9a34642b649aa1b6be2f693 |
| 出典メモ | uspto-grants-2014_02 |