関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | Ethyl 5-(4-(trifluoromethyl)phenyl)isoxazole-3-carboxylate | HCID 22064085 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Ethyl 4-chloro-5-(4-(trifluoromethyl)phenyl)isoxazole-3-carboxylate | HCID 67121079 | 86.2% |
反応手順
To a suspension of ethyl 5-(4-(trifluoromethyl)phenyl)isoxazole-3-carboxylate (3.3 g, 11.6 mmol) in acetic acid (60 mL) was added N-chlorosuccinimide (3.1 g, 23.2 mmol). Upon heating to 75° C., a homogenous solution formed. After heating for 16 hours a further portion of N-chlorosuccinimide (1.5 g, 11.2 mmol) was added and the reaction was heated at 75° C. for another 16 hours. After cooling to ambient temperature, the reaction mixture was poured over ice. The white crystals which formed were collected by vacuum filtration and purified by silica gel chromatography, eluting with dichloromethane to obtain the title compound (3.2 g, 10.0 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08211927B2 |
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| 出典データセット | uspto-grants-2012_07 |
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| ORD ID | ord-79638dfe31f5444583a6460c472f400a |
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| 出典メモ | uspto-grants-2012_07 |
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