반응 #11719

반응 방정식

4-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-4-oxo-butyric acid ethyl ester

tetrahydrofuran

methanol

lithium hydroxide monohydrate

→

title compound

수율 91.7%

4-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-4-oxo-butyric acid

수율 91.7%

용매

water

반응 조건

후처리

1. 1
   농축concentrated in vacuo
2. 2
   workup.DISSOLUTIONThe crude product was dissolved in ethyl acetate
3. 3
   세척washed with 1 M hydrochloric acid
4. 4
   건조The organics were dried over magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo

실험 절차

To a solution of 4-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-4-oxo-butyric acid ethyl ester (0.082 g, 0.16 mmol) in 2:2:1 tetrahydrofuran:methanol:water(1.5 mL) was added lithium hydroxide monohydrate (0.34 g, 0.79 mmol). The resulting solution was stirred 12 hours at ambient temperature, then concentrated in vacuo. The crude product was dissolved in ethyl acetate and washed with 1 M hydrochloric acid. The organics were dried over magnesium sulfate, filtered and concentrated in vacuo to give the title compound (0.072 g, LRMS: 489.4, 491.4).

출처