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HRID 229936作成日:2026年10月25日

Hydrochloric Acid → N,N-Dimethyl-2-cyano-3-difluoromethoxyphenylsulfonamide

https://huagongshe.com/reaction/229936

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DimethylamineHCID 674—
反応物Sodium CarbonateHCID 10340—
反応物2-Cyano-3-difluoromethoxyphenylsulfonyl chlorideHCID 58100767—
溶媒WaterHCID 962—
溶媒TetrahydrofuranHCID 8028—
生成物N,N-Dimethyl-2-cyano-3-difluoromethoxyphenylsulfonamideHCID 11492812—

反応手順

To a solution of 0.65 g (2.4 mmol) of purified 2-cyano-3-difluoromethoxyphenylsulfonyl chloride in 20 ml of tetrahydrofuran a solution of 274 mg (2.4 mmol) of dimethylamine and 510 mg of sodium carbonate in 15 ml of water was added at room temperature. The reaction mixture was stirred at room temperature for 5 minutes before water was added. The aqueous phase was acidified to pH=1 using hydrochloric acid (10% strength by weight, aqueous solution). The aqueous phase was then extracted three times with dichloromethane. The combined organic extracts were dried over sodium sulfate and filtered. The filtrate was concentrated in vacuo and the resulting residue was triturated with methyl tert-butyl ether. Yield: 0.53 g (79% of theory) of the title compound having a melting point of 100-102° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07563921B2
出典データセットuspto-grants-2009_07
ORD IDord-60568919defe4ae49f601bc989e84393
出典メモuspto-grants-2009_07