関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Fluoro-4-nitrophenol | HCID 9825 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4,5-Dichloropyrrolo[2,1-f][1,2,4]triazine | HCID 21081669 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Chloro-4-(2-fluoro-4-nitrophenoxy)pyrrolo[2,1-f][1,2,4]triazine | HCID 21081699 | 71.5% |
反応手順
A mixture of 4,5-dichloropyrrolo[2,1-f][1,2,4]triazine (3.73 g, 19.8 mmol), 2-fluoro-4-nitrophenol (3.43 g, 21.8 mmol) and potassium carbonate (5.47 g, 39.6 mmol) in DMF (100 mL) was stirred at 60° C. for 1 h. After cooling to rt, the reaction was filtered through a short plug of silica gel with ethyl acetate and then concentrated in vacuo. The crude product was purified by recrystallization from ethyl acetate/hexanes (1:1) to give the title compound (4.37 g, 71%) as a white solid. 1H NMR (CDCl3) δ 8.22–8.17 (m, 2H), 7.92 (s, 1H), 7.77 (d, 1H, J=2.8 Hz), 7.58 (t, 1H, J=7.2 Hz), 6.87 (d, 1H, J=3.2 Hz); MS(ESI+) m/z 309.3 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07173031B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-beb7dbbf2c0a427cae54be6596f241ff |
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| 出典メモ | uspto-grants-2007_02 |
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