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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

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物TriethylamineHCID 8471—
反応物2-(Trifluoromethyl)benzoyl chlorideHCID 67561—
反応物(2E)-2-[3-chloro-5-(trifluoromethyl)-2-pyridinyl]-2-(cyclopropylmethoxyimino)ethanamineHCID 118071502—
溶媒DichloromethaneHCID 6344—
生成物(Z)-N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(cyclopropylmethoxyimino)ethyl]-2-(trifluoromethyl)benzamideHCID 11807151294.7%

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US09434684B2
出典データセットuspto-grants-2016_09
ORD IDord-ce3353de775042cdbc0a243cba669183
出典メモuspto-grants-2016_09