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HRID 1962365作成日:2026年10月26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/1962365

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 was added 3 g of sodium methoxide. The reaction mixture was heated to 65° C. and stirred for 5 hours. The reaction mixture was poured into brine, neutralized and extracted with ethyl acetate. The organic phase was washed with brine, dried with sodium sulfate, filtered and concentrated. The residue was 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 (compound C8) as a solid, mp: >250° 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-1500ab0208b248229a0d804bfbf65ad4
出典メモuspto-grants-2013_04