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HRID 1962364作成日:2026年10月26日

Sulfuric Acid → 1-Ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester

https://huagongshe.com/reaction/1962364

反応式

関与物質

役割名称HCID仕込み量
反応物Sulfuric AcidHCID 1118—
反応物Sodium CarbonateHCID 10340—
反応物N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamideHCID 59614586—
溶媒MethanolHCID 887—
生成物1-Ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl esterHCID 59614592—

反応手順

1.4 ml of concentrated sulfuric acid was slowly added to a solution of 4.3 g of N-(4-cyano-1-ethoxy-piperidin-4-yl)-2-(2,4,6-trimethyl-phenyl)-acetamide in 11 ml of methanol. After stirring 20 hours under reflux, the reaction mixture was allowed to cool down to room temperature and diluted with ice water. Sodium carbonate was added and the aqueous phase was extracted with ethyl acetate. The organic phase was dried over sodium sulfate, filtered and concentrated. Chromatography (dichloromethane+1% of ethanol) gave 3.2 g of 1-ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester as a solid, mp: 131-132° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08415369B2
出典データセットuspto-grants-2013_04
ORD IDord-9b3f66b345844f11a12c2b3b771ed926
出典メモuspto-grants-2013_04