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HRID 508404作成日:2026年10月24日

Hydrochloric Acid → HCID 56644527、化合物

https://huagongshe.com/ja/reaction/508404

反応式

関与物質

役割名称HCID仕込み量
反応物Hydrochloric AcidHCID 313—
反応物Potassium CarbonateHCID 11430—
反応物3-Chloro-4-(trifluoromethyl)phenolHCID 13609147—
反応物4-(Bromomethyl)-2,5-difluoro-N-(methylsulfonyl)benzamideHCID 66667111—
溶媒Dimethyl SulfoxideHCID 679—
生成物HCID 56644527HCID 5664452756.3%

反応手順

A solution of 3-chloro-4-(trifluoromethyl)phenol (Preparation 5, 50 mg, 0.26 mmol), 4-(bromomethyl)-2,5-difluoro-N-(methylsulfonyl)benzamide (Preparation 4, 84 mg, 0.26 mmol) and potassium carbonate (71 mg, 0.51 mmol) in dimethyl sulfoxide (5 mL) was stirred at room temperature for 16 hours. A 2M aqueous solution of hydrogen chloride was added to the reaction mixture. The resulting precipitate was filtered, washed with diethyl ether (5 mL) and dried. The material was purified by reverse phase column chromatography (12 g C-18 biotage cartridge; eluents: MeCN+0.1% formic acid, and H2O+0.1% formic acid; Gradient: 30% MeCN, followed by gradient to 100% MeCN, 100% MeCN. Fractions containing product were combined and concentrated in vacuo to afford the title compound as a colourless solid (65 mg, 56%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09096500B2
出典データセットuspto-grants-2015_08
ORD IDord-0d6188b512ea48448d6dfeff5f43094f
出典メモuspto-grants-2015_08