関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1H-Indazol-5-ol | HCID 101438 | — |
| 反応物 | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1h-Indazole,5-(2-fluoro-4-nitrophenoxy)- | HCID 17979352 | — |
反応手順
5.00 g (37.3 mmol) of 5-hydroxyindazole are dissolved in 40 ml of anhydrous DMF. 5.93 g (37.3 mmol) of 3,4-difluoronitrobenzene and 5.15 g (37.3 mmol) of potassium carbonate are added, and the mixture is stirred at 40° C. overnight. For work-up, the mixture is filtered off with suction through kieselguhr, diluted with water and extracted three times with ethyl acetate. The combined organic phases are washed 1× with saturated aqueous sodium chloride solution, dried over sodium sulfate and concentrated using a rotary evaporator. The residue is chromatographed twice on silica gel using cyclohexane/ethyl acetate 3:1→1:1→1:2 and then purified by preparative HPLC.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737153B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-148ed9b344d04550bc6dd240a54fb706 |
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| 出典メモ | uspto-grants-2010_06 |
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