HRID131411
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Stir a solution of (S)-2-(3-ethoxycarbonylpropyl)-piperazine-1,4-dicarboxylic acid di-tert-butyl ester (0.739 g, 1.84 mmol) in MeOH add 1.0 N NaOH (2.13 mL) and continue stirring overnight. Concentrate the mixture under reduced pressure, dilute with H2O (40 mL) and wash with Et2O (3×30 mL). Acidify the aqueous layer with 10% NaHSO4 (20 mL) and extract with EtOAc (3×50 mL). Dry the organic layer with Na2SO4 filter, concentrate under reduced pressure and place the residue under vacuum to give the title compound: white solid (0.618 g), mass spectrum (m/e):373.07 (M+H).
WORKUP
后处理
- concentrationConcentrate the mixture under reduced pressure
- additiondilute with H2O (40 mL)
- washwash with Et2O (3×30 mL)
- extractionextract with EtOAc (3×50 mL)
- dry with materialDry the organic layer with Na2SO4
- filtrationfilter
- concentrationconcentrate under reduced pressure and place the residue under vacuum