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HRID 2359302作成日:2026年10月27日

Water → 4-Bromo-2-chloro-1-(difluoromethoxy)benzene

https://huagongshe.com/reaction/2359302

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4-Bromo-2-chlorophenolHCID 19859—
反応物Sodium chlorodifluoroacetateHCID 2734985—
溶媒DimethylformamideHCID 6228—
生成物4-Bromo-2-chloro-1-(difluoromethoxy)benzeneHCID 4631153867.2%

反応手順

4-bromo-2-chlorophenol (1.0 g, 4.8 mmol) was dissolved in DMF (35 ml) and water (5 ml) was added followed by sodium chloro(difluoro)acetate (2.0 g, 12 mmol) and cesium carbonate (3.1 g, 9.6 mmol). The mixture was stirred for 15 minutes at room temperature and then heated to 100° C. for 2 hours under nitrogen. The mixture was partitioned between water (50 ml) and tBuOMe (50 ml). The organic phase was separated, washed brine, dried over sodium sulphate, filtered, and concentrated in vacuo to give a crude product. The crude product was purified by silica gel chromatography eluting with 0-30% EtOAc in heptanes to give a title compound (0.83 g, 67% yield) as colourless oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08685977B2
出典データセットuspto-grants-2014_04
ORD IDord-01fedac981e3476fb5b29d048fe4228b
出典メモuspto-grants-2014_04