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HRID 1022377作成日:2026年10月27日

Sodium Methoxide → 8-Ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one

https://huagongshe.com/reaction/1022377

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium MethoxideHCID 10942334—
反応物1-Ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl esterHCID 59614592—
溶媒DimethylformamideHCID 6228—
溶媒Sodium chloride; waterHCID 57417360—
生成物8-Ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-oneHCID 5961458124.3%

反応条件

温度65 °C

反応手順

To a solution of 2.3 g of 1-ethoxy-4-[2-(2,4,6-trimethyl-phenyl)-acetylamino]-piperidine-4-carboxylic acid methyl ester in 26 ml of dimethylformamide is added 3 g of sodium methoxide. The reaction mixture is heated to 65° C. and stirred for 5 hours. The reaction mixture is poured into brine, neutralized and extracted with ethyl acetate. The organic phase is washed with brine, dried with sodium sulfate, filtered and concentrated. The residue is subjected to column chromatography (heptane/ethyl acetate 2:1) to yield 510 mg of 8-ethoxy-4-hydroxy-3-(2,4,6-trimethyl-phenyl)-1,8-diaza-spiro[4.5]dec-3-en-2-one as a solid, mp: >250° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08722578B2
出典データセットuspto-grants-2014_05
ORD IDord-ffdf53a0b4db4e33b98754217bd6a43d
出典メモuspto-grants-2014_05