HRID2371169
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
tert-Butyl (3S)-3-{[4-(anilinocarbonyl)piperazin-1-yl]methyl}piperidine-1-carboxylate (4.0 g) was added to a mixture of dichloromethane (20 ml) and TFA (20 ml) and the reaction mixture stirred for 2 h. The solvent was removed in-vacuo and the residue dissolved in dichloromethane (20 ml) and subsequently poured into hydrochloric acid solution (1N, 20 ml). The aqueous layer was basified using potassium carbonate and extracted with dichloromethane (3×15 ml). The organic layer was dried using a phase separation cartridge and the solvent removed under reduced pressure to afford the desired compound as a white foam white (2.0 g), which was used without further purification.
WORKUP
后处理
- customThe solvent was removed in-vacuo
- dissolutionthe residue dissolved in dichloromethane (20 ml)
- additionsubsequently poured into hydrochloric acid solution (1N, 20 ml)
- extractionextracted with dichloromethane (3×15 ml)
- customThe organic layer was dried
- customa phase separation cartridge
- customthe solvent removed under reduced pressure