반응 #11733

반응 방정식

3-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzylamino)-propionic acid methyl ester

lithium hydroxide monohydrate

→

title compound

3-(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzylamino)-propionic acid

용매

tetrahydrofuran

methanol

water

반응 조건

후처리

1. 1
   농축The reaction mixture was then concentrated in vacuo
2. 2
   workup.DISSOLUTIONthe resulting residue was dissolved in dichloromethane
3. 3
   workup.ADDITIONtreated with hydrogen chloride gas
4. 4
   세척The resulting white solid was washed with acetonitrile
5. 5
   세척The acetonitrile wash
6. 6
   농축was concentrated

실험 절차

To a solution of 3-(5-chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzylamino)-propionic acid methyl ester (0.035 g, 0.069 mmol) in tetrahydrofuran (0.2 mL), methanol (0.2 mL) and water (0.1 mL) was added lithium hydroxide monohydrate (0.015 g, 0.35 mmol). The reaction mixture was stirred at ambient temperature overnight. The reaction mixture was then concentrated in vacuo and the resulting residue was dissolved in dichloromethane and treated with hydrogen chloride gas. The resulting white solid was washed with acetonitrile. The acetonitrile wash was concentrated to give the title compound as its hydrochloride salt (0.010 g, LRMS: 490.3).

출처