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Sulfolane → 2-Fluoro-5-nitropyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfolane | HCID 31347 | — |
| 反応物 | 2-Chloro-5-nitropyridine | HCID 78308 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-Fluoro-5-nitropyridine | HCID 95264 | — |
反応手順
A mixture of 5-nitro-2-chloropyridine (2.0 g, 12.6 mmol) and anhydrous potassium fluoride (2.2 g, 38 mmol) in a combination of sulfalone (6 mL) and benzene (4 mL) was stirred at RT for 20 min. The benzene was then removed by distillation. The resulting mixture was heated at 150° C. for 12 h. The mixture was cooled to RT whereupon water (60 mL) was added. The desired product was separated from the solution via steam distillation. Extraction of the distillate with diethyl ether (2×10 mL) followed by drying (Na2SO4) and concentration gave 5-nitro-2-fluoropyridine as a water white oil (1.3 g, 73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06605725B2 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-949b3abdd77d4b8396530941a4ae092d |
| 出典メモ | uspto-grants-2003_08 |