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HRID 1484683作成日:2026年10月27日

Water → Benzenemethanol, 4-(difluoromethoxy)-2,6-difluoro-

https://huagongshe.com/reaction/1484683

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Cesium carbonateHCID 10796—
反応物Sodium chlorodifluoroacetateHCID 2734985—
反応物3,5-Difluoro-4-(hydroxymethyl)phenolHCID 22219975—
溶媒DimethylformamideHCID 6228—
溶媒Ethyl AcetateHCID 8857—
生成物Benzenemethanol, 4-(difluoromethoxy)-2,6-difluoro-HCID 6914094456%

反応条件

温度100 °C

反応手順

500 mg 3,5-difluoro-4-(hydroxymethyl)phenol (3.12 mmol, 1.0 eq.) were dissolved in DMF. 523 mg sodium chloro(difluoro)acetate (3.44 mmol, 1.1 eq.), 1.22 g cesium carbonate (3.75 mmo, 1.2 eq) and 0.20 mL water (10.9 mmol, 3.5 eq.) were added. The reaction mixture was stirred at 100° C. over night. The reaction mixture was divided between water and ethyl acetate. The aqueous layer was washed twice with ethyl acetate. The combined organic layers were washed with brine, dried over a silicon filter and concentrated in vacuo. The crude product was purified by flash chromatography to provide 161 mg (0.69 mmol, 22%) of the 56% pure target compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09422268B2
出典データセットuspto-grants-2016_08
ORD IDord-ccdc2f7392d948c583bacedff73d2af3
出典メモuspto-grants-2016_08