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HRID 3017作成日:2026年10月23日

Ethyl Acetate → 4-(Difluoromethoxy)benzonitrile

https://huagongshe.com/ja/reaction/3017

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl AcetateHCID 8857—
反応物4-CyanophenolHCID 13019—
反応物Sodium HydroxideHCID 14798—
反応物Sodium chlorodifluoroacetateHCID 2734985—
溶媒DimethylformamideHCID 6228—
生成物4-(Difluoromethoxy)benzonitrileHCID 273699041%

反応手順

4-Cyanophenol (0.50 g, 4.2 mmol, Aldrich), sodium chlorodifluoroacetate (0.77 g, 5 mmol, Alfa Products), and sodium hydroxide (0.20 g, 5 mmol) were combined in dry DMF (2 mL) under an atmosphere of argon. After stirring at 125°-130° C. for 5 h, the mixture was cooled to RT, ethyl acetate (50 mL) was added and the organic layer was washed twice with brine. The organic extract was dried (MgSO4), filtered and evaporated. The residue was purified by flash chromatography (silica gel, 25% ethyl acetate/hexanes) to provide a white solid. The solid was sublimed (1 mm Hg, 23° C.) to provide the title compound as colorless crystals (0.29 g, 41%). mp 33°-35° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05731477
出典データセットuspto-grants-1998_03
ORD IDord-9878f8a1a69f4990b1191065d489c660
出典メモuspto-grants-1998_03