反应详情

Into a stirred, room temperature solution of (S)-2-(4-methoxybutyl)-piperazine-1,4-dicarboxylic acid di-tert-butyl ester (0.198 g, 0.53 mmol) in CH2Cl2 (2.6 mL), add TFA (2.6 mL) and stir for 2 h. Concentrate the mixture under reduced pressure, dilute with H2O and load onto an SCX column (10 g). Wash the resin with H2O (3×100 mL), MeOH (3×100 mL) and elute the product with 2 M NH3 in MeOH (3×100 mL). Concentrate the purified fractions under reduced pressure and azeotrope the residue with CH2Cl2/hexanes (1:2). Place the residue under vacuum to give the title compound: orange crystals (0.093 g), mass spectrum (m/e):173.4 (M+H).

1. concentrationConcentrate the mixture under reduced pressure
2. additiondilute with H2O and load onto an SCX column (10 g)
3. washWash the resin with H2O (3×100 mL), MeOH (3×100 mL)
4. washelute the product with 2 M NH3 in MeOH (3×100 mL)
5. concentrationConcentrate the purified fractions under reduced pressure