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HRID 55995作成日:2026年10月25日
Water → (Z)-N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(cyclopropylmethoxyimino)ethyl]-2-(trifluoromethyl)benzamide
https://huagongshe.com/reaction/55995
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(Trifluoromethyl)benzoyl chloride | HCID 67561 | — |
| 反応物 | (2E)-2-[3-chloro-5-(trifluoromethyl)-2-pyridinyl]-2-(cyclopropylmethoxyimino)ethanamine | HCID 118071502 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (Z)-N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(cyclopropylmethoxyimino)ethyl]-2-(trifluoromethyl)benzamide | HCID 118071512 | 94.7% |
反応手順
In a solution of 65 mg of (E)-2-amino-1-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]ethanone-O-(cyclopropylmethyl)oxime and 32 mg of triethylamine in 2 ml of dichloromethane, 39 mg of 2-(trifluoromethyl)benzoyl chloride was added dropwise with stirring under cooling with ice, and after the addition, the mixture was stirred at room temperature for another 1 hour. After completion of the reaction, the reaction mixture was mixed with 2 ml of water and extracted with dichloromethane (2 ml×1), the resulting organic layer was dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by preparative medium pressure liquid chromatography (preparative medium pressure chromatograph: YFLC-Wprep manufactured by Yamazen Science, Inc.) using ethyl acetate-hexane (with a gradient of from 2:18 to 5:15) as the eluent to obtain 85 mg of the desired product as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434684B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-ce3353de775042cdbc0a243cba669183 |
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| 出典メモ | uspto-grants-2016_09 |
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