反应详情

温度

25 °C

A solution of 1-(tert-butoxycarbonyl)-4-[{N-(3-(trifluoromethyl)benzoyl)glycyl}aminomethyl]piperidine (2.29 g, 5.16 mmol) in CH3OH (40 mL) was treated with 1 N HCl-Et2O (55 mL). The reaction mixture was stirred at 25° C. for 15 h and the solvent was removed under reduced pressure. 2 N aqueous NaOH solution (100 mL) was added to the reaction mixture and the mixture was extracted with EtOAc (3×100 mL). The combined extracts were washed with brine and dried (K2CO3). The solvent was removed under reduced pressure to afford a white solid which was purified by column chromatography (SiO2, CH3OH/CH2Cl2/Et3N=7/6/1)) to give 4-[{N-(3-(trifluoromethyl)benzoyl)glycyl}aminomethyl]piperidine as a white solid (1.27 g, 72%): The purity was determined by RPLC/MS (98%); ESI/MS m/e 344.1 (M++H, C16H20F3N3O2).

1. customthe solvent was removed under reduced pressure
2. addition2 N aqueous NaOH solution (100 mL) was added to the reaction mixture
3. extractionthe mixture was extracted with EtOAc (3×100 mL)
4. washThe combined extracts were washed with brine
5. dry with materialdried (K2CO3)
6. customThe solvent was removed under reduced pressure
7. customto afford a white solid which
8. customwas purified by column chromatography (SiO2, CH3OH/CH2Cl2/Et3N=7/6/1))