関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,1,1-Trifluoro-2-iodoethane | HCID 67709 | — |
| 反応物 | 4-Chloro-2-fluorophenol | HCID 181975 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Chloro-2-fluoro-1-(2,2,2-trifluoroethoxy)benzene | HCID 59506748 | — |
反応手順
To 4-Chloro-2-fluoro-phenol (521, 5.0 g, 0.034 mol) in methanol (50.0 mL) was added potassium fluoride (2.2 g, 0.038 mol). The solvent was removed. The resulting salt was added to N,N-dimethylformaldehyde (25 mL), followed by adding 1,1,1-trifluoro-2-iodo-ethane (8.60 g, 40.9 mmol). The reaction was stirred at 50° C. overnight. The reaction was poured into water and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 20% ethyl acetate in hexane to give colorless oil (522, 2.0 g, 26%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08143271B2 |
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| 出典データセット | uspto-grants-2012_03 |
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| ORD ID | ord-6f27ff4e3db344cea051d96aa76bea9a |
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| 出典メモ | uspto-grants-2012_03 |
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