関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 2-(2-Bromo-4-chlorophenoxy)cyclopentanone | HCID 58566778 | — |
| 触媒 | Methyltriphenyliphosphonium bromide | HCID 74505 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-4-chloro-1-(2-methylenecyclopentyloxy)benzene | HCID 58566637 | 58.2% |
反応手順
To the mixture of methyl triphenylphosphonium bromide (16.0 g, 44.8 mmol) in anhydrous tetrahydrofuran (125 mL) at 0° C. under nitrogen was added portion wise the potassium tert-butoxide (5.0 g, 44.8 mmol). After stirring at 0° C. for 30 minutes, the mixture of 2-(2-bromo-4-chlorophenoxy)cyclopentanone (516B) (10.8 g, 37.3 mmol) in tetrahydrofuran (40 mL) was added slowly. The resulting mixture was stirred at room temperature under nitrogen for 3 hours. The reaction mixture was quenched with water and extracted with ethyl acetate. The organic phase was washed with water, brine, dried with sodium sulfate and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel (5-10% EtOAc in hexanes) to provide 2-bromo-4-chloro-1-(2-methylenecyclopentyloxy)benzene (517) (6.2 g, 58.2%) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476308B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-e800d57c0eec4c0587e7e28be28536f3 |
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| 出典メモ | uspto-grants-2013_07 |
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