関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 5-Fluoro-4-methyl-2-nitropyridine | HCID 59184740 | — |
| 反応物 | HCID 178516507 | HCID 178516507 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-4-(4-methyl-6-nitropyridin-3-yloxy)pyridine | HCID 86641689 | 62.5% |
反応手順
A mixture of 5-fluoro-4-methyl-2-nitropyridine (0.8 g, 5.12 mmol), 4-hydroxy-2-chloropyridine (0.996 g, 7.69 mmol) and K2CO3 (0.708 g, 5.12 mmol) in DMF (10 mL) was heated at 80° C. for 4 h. The mixture was cooled to RT, poured onto water, extracted with EtOAc (2×) and the combined organics were washed with brine, dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (EtOAc/Hex) to afford 5-((2-chloropyridin-4-yl)oxy)-4-methyl-2-nitropyridine (850 mg, 62%) as an off-white solid. MS (ESI) m/z: 266.0 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09309224B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-fdf4fb60fcbe4145ab6503576c355e6a |
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| 出典メモ | uspto-grants-2016_04 |
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