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Hydrochloric Acid → 2-Chloro-5-iodo-3-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | 2-Amino-5-iodo-3-nitropyridine | HCID 3384468 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 生成物 | 2-Chloro-5-iodo-3-nitropyridine | HCID 1514294 | 36% |
反応手順
5-iodo-3-nitro-2-aminopyridine (2.511 g, 9.48 mmol) and concentrated HCl (20 mL) were stirred at room temperature for ten minutes. Sodium nitrite (13 g, 188 mmol) was then slowly added followed by CuCl (1.0 g, 10 mmol). Stirring continued overnight. The mixture was poured into 1:1 NH4OH:H2O, extracted with ethyl acetate, dried over sodium sulfate, then concentrated. The crude residue was purified by flash chromatography using 9:1 hexane:ethyl acetate to yield 5-iodo-3-nitro-2-chloropyridine (984 mg, 36%) as a colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07615567B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-9c8d146798a34822a21c69430887e465 |
| 出典メモ | uspto-grants-2009_11 |