関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1-Fluoro-2-nitrobenzene | HCID 73895 | — |
| 反応物 | Methyl 5-fluoro-2-hydroxybenzoate | HCID 2783186 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 5-fluoro-2-(2-nitrophenoxy)benzoate | HCID 59783776 | 84.4% |
反応手順
Methyl 5-fluoro-2-hydroxybenzoate (2.65 g, 15.6 mmo.) and 1-fluoro-2-nitrobenzene (2.02 g, 14.2 mmol) were dissolved in acetonitrile (30 mL) and cesium carbonate (6.10 g, 18.7 mmol) was added. The reaction mixture was stirred at 80° C. for 60 hours. The mixture was cooled down to room temperature and poured into ethyl acetate. This organic mixture was washed with water and brine, dried over sodium sulfate, filtered and evaporated. The crude was purified by flash chromatography with 10-20% ethyl acetate in hexanes and triturated in ethanol to afford the title compound 18 (3.49 g, 84%) as white solid. LRMS (ESI): (calc) 291.05. (found) 292.2 (MS)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09193749B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-2db8f05811d54b7591401200770970a1 |
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| 出典メモ | uspto-grants-2015_11 |
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