関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 4-Bromo-2-chlorophenol | HCID 19859 | — |
| 反応物 | 2-Chloro-2,2-difluoroacetophenone | HCID 238296 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 4-Bromo-2-chloro-1-(difluoromethoxy)benzene | HCID 46311538 | 52% |
反応手順
A solution of 4-bromo-2-chlorophenol (830 mg) and a 30% potassium hydroxide solution (16 mL) in acetonitrile (16 mL) was cooled to −78° C. 2-Chloro-2,2-difluoroacetophenone (2.95 mL) was added and the mixture was stirred at 80° C. for 40 hours. The reaction solution was cooled to room temperature and extracted with diethyl ether. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1→10:1) to give 4-bromo-2-chloro-1-(difluoromethoxy)benzene as a colorless oil (533 mg, 52%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08822503B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-1c82bc8a453045e1bd8067176806964e |
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| 出典メモ | uspto-grants-2014_09 |
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