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HRID 1364422作成日:2026年10月27日

Ethyl Acetate → 2-Fluoro-6-(2,3,5-trifluorobenzyloxy)-benzonitrile

https://huagongshe.com/reaction/1364422

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Sodium hydrideHCID 24758—
反応物2,6-DifluorobenzonitrileHCID 74695—
反応物2,3,5-Trifluorobenzyl alcoholHCID 2777030—
溶媒DimethylformamideHCID 6228—
生成物2-Fluoro-6-(2,3,5-trifluorobenzyloxy)-benzonitrileHCID 6692422672.9%

反応手順

To a cold (ice water) suspension of sodium hydride (407 mg; 10 mmol) in anhydrous DMF (4 mL) is added a solution of 2,3,5-trifluorobenzyl alcohol (1.62 g; 10 mmol) in anhydrous DMF (5 mL) over 10 minutes. After allowing to room temperature over 1 hour, this solution is added to a cold (ice water) stirred solution of 2,6-difluorobenzonitrile (1.56 gm; 11 mmol) in anhydrous DMF (5 mL), and allowed to room temperature over 3 hours. TLC (25% EA/Hex) was incomplete so the reaction was continued at room temperature for an additional 2 hours. The reaction mixture is poured into ice water with vigorous stirring and the resulting solid is filtered, washed with water, and dried under vacuum at 40° C. for 4.5 hours to give 2.05 grams of 2-fluoro-6-(2,3,5-trifluorobenzyloxy)-benzonitrile.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07888366B2
出典データセットuspto-grants-2011_02
ORD IDord-421cc3f4908147949b751f0504a7ff94
出典メモuspto-grants-2011_02