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HRID 56014作成日:2026年10月24日

Pyridine → N-[2-(3,5-dichloropyridin-2-yl)-2-(tert-butoxyimino)ethyl]-2-(trifluoromethyl)benzamide

https://huagongshe.com/ja/reaction/56014

反応式

関与物質

役割名称HCID仕込み量
反応物PyridineHCID 1049—
反応物O-tert-butylhydroxylamine hydrochlorideHCID 2777906—
反応物N-[2-(3,5-dichloropyridin-2-yl)-2-oxoethyl]-2-(trifluoromethyl)benzamideHCID 118071552—
溶媒EthanolHCID 702—
生成物N-[2-(3,5-dichloropyridin-2-yl)-2-(tert-butoxyimino)ethyl]-2-(trifluoromethyl)benzamideHCID 13173689287.1%

反応条件

温度70 °C

反応手順

To a solution of 200 mg of the N-[2-(3,5-dichloropyridin-2-yl)-2-oxoethyl]-2-(trifluoromethyl)benzamide prepared in Step 3 in Synthetic Example 10 and 199 mg of O-(tert-butyl)hydroxylamine hydrochloride in 2.6 ml of ethanol, 167 mg of pyridine was added, and the mixture was stirred at 70° C. for 18 hours. After completion of the reaction, the solvent was evaporated under reduced pressure, the resulting residue was mixed with 2 ml of water and extracted with ethyl acetate (2 ml×2), the resulting organic layers were combined, 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 silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 5:95 to 50:50) as the eluent to obtain 207 mg of the desired product as a colorless resinous substance.

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-1293a59b7a6a4dea976cc614e1476dda
出典メモuspto-grants-2016_09