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HRID 1641464作成日:2026年10月27日

Sodium Sulfate → 3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamide

https://huagongshe.com/reaction/1641464

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium SulfateHCID 24436—
反応物Potassium tert-butoxideHCID 23665647—
反応物2-amino-5-chloro-N-(1-cyclopropylethyl)benzamideHCID 43533096—
反応物S-benzyl 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbothioateHCID 86639908—
溶媒Dimethyl SulfoxideHCID 679—
溶媒WaterHCID 962—
生成物3-bromo-N-(4-chloro-2-(1-cyclopropylethylcarbamoyl)phenyl)-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxamideHCID 6673619341.9%

反応手順

0.85 g of anhydrous sodium sulfate was added to a mixed solution comprising 0.24 g of 2-amino-5-chloro-N-(1-cyclopropylethyl)benzamide, 0.41 g of S-benzyl 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbothioate and 5 ml of dimethyl sulfoxide at room temperature, followed by stirring for 5 minutes, and 0.14 g of potassium tert-butoxide was added, followed by reaction at room temperature for 1 hour. The reaction liquid was slowly added to water, the mixed liquid was subjected to extraction with ethyl acetate, and the organic layer was washed with a sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1 to 7.5/2.5) to obtain 0.22 g of the desired product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08115006B2
出典データセットuspto-grants-2012_02
ORD IDord-36f05a2a6bec4b3fb2a0c9c96e1054e3
出典メモuspto-grants-2012_02