関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl fluoroacetate | HCID 9988 | — |
| 反応物 | HCID 178478998 | HCID 178478998 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Ammonium Chloride | HCID 25517 | — |
| 生成物 | 1-(2,4-Dichloro-phenyl)-3-fluoro-propan-2-one | HCID 86679079 | 49% |
反応手順
To a stirred solution of ethyl fluoroacetate (0.33 ml; 3.3 mmol) in dry diethyl ether (3.3 ml) under argon at −76° C. was added dropwise a 0.25 M solution of 2,4-dichlorobenzylmagnesium chloride in diethyl ether (20 ml; 5 mmol). The suspension was stirred at −60° C. during 5 h. The mixture was poured in ammonium chloride sat. solution and extracted three times with diethylether. Organics were combined, dried over sodium sulfate and evaporated to a resin which was subject to flash chromatography (eluant: c-hexane/ethyl acetate 99:1 to 70:30) to afford 0.36 g (49% of theory) of 1-(2,4-dichloro-phenyl)-3-fluoro-propan-2-one as a pale yellow solid (melting point: 48-52° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08552049B2 |
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| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-dc0682f2f4d54d288d87e16977c17797 |
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| 出典メモ | uspto-grants-2013_10 |
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