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HRID 2080463作成日:2026年10月26日

Diglycolamine → 2-[2-[5-Chloro-4-[(4-chlorophenylthio)(2,5-difluorophenyl)methyl]pyridin-2-ylamino]ethoxy]ethanol

https://huagongshe.com/reaction/2080463

反応式

関与物質

役割名称HCID仕込み量
反応物DiglycolamineHCID 13578—
反応物1,4-DioxaneHCID 31275—
反応物2,5-Dichloro-4-[(4-chlorophenylthio)-(2,5-difluorophenyl)methyl]pyridineHCID 23114567—
溶媒Dichloromethane methanolHCID 21226129—
生成物2-[2-[5-Chloro-4-[(4-chlorophenylthio)(2,5-difluorophenyl)methyl]pyridin-2-ylamino]ethoxy]ethanolHCID 2311465335%

反応手順

A dioxane (1.5 ml) solution of the 2,5-dichloro-4-[(4-chlorophenylthio)(2,5-difluorophenyl)methyl]pyridine (210 mg, 0.504 mmol) obtained in Example 54 and 2-(2-aminoethoxy)ethanol (400 μl) was heated at 120° C. for 3 days in a sealed tube. The reaction mixture was cooled to room temperature and then, concentrated under reduced pressure. Water was added to the residue thus obtained, followed by extraction with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to silica gel column chromatography. The fraction obtained from the 30% methanol/methylene chloride eluate was concentrated under reduced pressure to give the title compound (85 mg, 0.175 mmol, 35%) as a colorless oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07932271B2
出典データセットuspto-grants-2011_04
ORD IDord-296c5fff487548418df8b5da8b434e9f
出典メモuspto-grants-2011_04