関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phenol, 2-chloro-4-fluoro-5-nitro- | HCID 158655 | — |
| 反応物 | Cyclopentyl 4-methylbenzene-1-sulfonate | HCID 317685 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-Fluoro-4-chloro-5-cyclopentyloxynitrobenzene | HCID 19374470 | 92.6% |
反応手順
A solution of 2-fluoro-4-chloro-5-hydroxynitrobenzene (7.1 g, 37.1 mmol) and potassium carbonate (5.1 g, 37.1 mmol) in acetonitrile (300 ml) was stirred for 2 hours at a refluxing temperature. Cyclopentyl p-toluenesulfonate (10.3 g, 40.8 mmol) was added thereto, followed by stirring further for 2 hours under refluxing. After completion of the reaction, the solvent was distilled off under reduced pressure from the reaction mixture, in hydrochloric acid (300 ml) was added thereto, and the mixture was extracted with ethyl acetate (100 ml×3 times). The organic layer was washed with an aqueous solution of sodium bicarbonate and water, dried, and the solvent was distilled off under reduced pressure to obtain 2-fluoro-4-chloro-5-cyclopentyloxynitrobenzene as a yellow solid (8.93 g, 34.3 mmol, 92.6% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424277 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-0b1ea39f652a4ec0b1ad722b5587f73d |
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| 出典メモ | uspto-grants-1995_06 |
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