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Hydrogen Bromide → 2-Bromo-5-iodo-3-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 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 | — |
| 生成物 | 2-Bromo-5-iodo-3-nitropyridine | HCID 18619785 | 23% |
反応手順
5-iodo-3-nitro-2-aminopyridine (5.6 g, 21.1 mmol) and concentrated HBr (60 mL) were stirred at room temperature for ten minutes. Sodium nitrite (11.7 g, 170 mmol) was then slowly added followed by CuBr (3.9 g, 27.2 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-bromopyridine (1.618 g, 23%) 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-68c9d6171e4c4c63aa75cb8747ad4930 |
| 出典メモ | uspto-grants-2009_11 |