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HRID 11697作成日:2026年10月24日

Ethyl nitroacetate → 3-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-2-nitro-propionic Acid Ethyl Ester

https://huagongshe.com/ja/reaction/11697

反応式

関与物質

役割名称HCID仕込み量
反応物Ethyl nitroacetateHCID 69379—
反応物Sodium BicarbonateHCID 516892—
反応物2-[4-Chloro-2-(chloromethyl)phenoxy]-1-{(2R,5S)-4-[(4-fluorophenyl)methyl]-2,5-dimethylpiperazin-1-yl}ethan-1-oneHCID 23405842—
触媒Tetrabutylammonium IodideHCID 67553—
溶媒DimethylformamideHCID 6228—
生成物3-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-2-nitro-propionic Acid Ethyl EsterHCID 8659116747%

反応条件

温度60 °C

反応手順

To nitro-acetic acid ethyl ester (0.32 g, 2.39 mmol), sodium bicarbonate (0.10 g, 1.19 mmol) and tetrabutyl ammonium iodide (0.088 g, 0.24 mmol) in dimethyl formamide (5 ml) was added 2-(4-chloro-2-chloromethyl-phenoxy)-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (0.52 g, 1.19 mmol). After 1 hour of heating at 60° C. the reaction was concentrated and then diluted with methylene chloride. After washing with aqueous saturated sodium bicarbonate and saturated sodium chloride the organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (0.30 g).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07098212B2
出典データセットuspto-grants-2006_08
ORD IDord-34e48198b45f4c59b72297ec362acb71
出典メモuspto-grants-2006_08