반응 #11793

반응 방정식

nitro-acetic acid ethyl ester

sodium bicarbonate

2-(4-chloro-2-chloromethyl-phenoxy)-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone

→

title compound

수율 47.0%

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

수율 47.0%

용매

dimethyl formamide

반응 조건

후처리

1. 1
   농축was concentrated
2. 2
   workup.ADDITIONdiluted with methylene chloride
3. 3
   세척After washing with aqueous saturated sodium bicarbonate and saturated sodium chloride the organic layer
4. 4
   건조was dried over magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo

실험 절차

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).

출처