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HRID 81639作成日:2026年10月25日

Dimethylformamide → 5-[2-(1,3-Dioxolan-2-yl)ethoxy]-2,3-difluoropyridine

https://huagongshe.com/reaction/81639

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Cesium carbonateHCID 10796—
反応物2-(2-Bromoethyl)-1,3-dioxolaneHCID 87776—
反応物5,6-Difluoropyridin-3-olHCID 68430860—
溶媒WaterHCID 962—
生成物5-[2-(1,3-Dioxolan-2-yl)ethoxy]-2,3-difluoropyridineHCID 6842976238.1%

反応条件

温度100 °C

反応手順

Cesium carbonate (33 g, 100 mmol) and 2-(2-bromoethyl)-1,3-dioxolane (12 g, 67 mmol) were added to an N,N-dimethylformamide suspension (30 ml) of 5,6-difluoropyridin-3-ol (8.8 g, 67 mmol), and stirred at 100° C. for 1 hour. The reaction solution was cooled to room temperature, water was added, and extracted with ethyl acetate. The organic layer was washed with saturated saline water, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:chloroform=1:1 to 0:1) to obtain 5-[2-(1,3-dioxolan-2-yl)ethoxy]-2,3-difluoropyridine (5.9 g, yield: 38%) as a pale yellow oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08846700B2
出典データセットuspto-grants-2014_09
ORD IDord-9e72d3e1c42543f1aabdb607ad88b529
出典メモuspto-grants-2014_09