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HRID 2274602作成日:2026年10月25日

Hydrochloric Acid → 2-(4-Chloro-3-dibutylcarbamoyl-5-methyl-pyrazol-1-yl)-5-methoxy-benzoic acid

https://huagongshe.com/reaction/2274602

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 HydroxideHCID 14797—
反応物Dichloromethane methanolHCID 21226129—
反応物4-Chloro-1-(2-cyano-4-methoxy-phenyl)-5-methyl-1H-pyrazole-3-carboxylic acid dibutylamideHCID 89649586—
溶媒EthanolHCID 702—
溶媒WaterHCID 962—
生成物2-(4-Chloro-3-dibutylcarbamoyl-5-methyl-pyrazol-1-yl)-5-methoxy-benzoic acidHCID 8964705739%

反応手順

A mixture of 4-Chloro-1-(2-cyano-4-methoxy-phenyl)-5-methyl-1H-pyrazole-3-carboxylic acid dibutylamide (1.3 g, 3.2 mmol) and potassium hydroxide (1.2 g, 21 mmol) in ethanol (5 mL) and water (5 mL) was microwaved at 150° C. for 90 minutes. The pH was adjusted to about 5 with aqueous HCl solution (15 N). The solvent was removed in vacuo. The crude material was eluted through a silica gel column with a 10 to 100% ethyl acetate/heptane and then 1 to 20% methanol/methylene chloride gradient to afford the title compound (0.53 g, 39% yield) as a white solid. MS (ESI) [m/e, (M+H)+]=422.4.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09126979B2
出典データセットuspto-grants-2015_09
ORD IDord-2490eb43b6b74ecead38bbed16fe40a0
出典メモuspto-grants-2015_09