HRID408022
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
To a solution of (25)-2-(benzyloxycarbonylamino)-4-(1-(tert-butoxycarbonyl)-3,3-dimethylpiperidin-4-ylamino)butanoic acid (3.59 g, 7.74 mmol) in DMF (20 mL) was added DIEA (4.1 mL, 23 mmol) and HBTU (3.5 g, 9.3 mmol). The mixture stirred at ambient temperature overnight. The mixture was poured into 1 N NaOH solution and extracted into ethyl acetate. The organic layer was washed with 1 N HCl solution and brine, dried over MgSO4, filtered and concentrated under vacuum. Flash chromatography (7:3 EtOAc:hexanes) gave tert-butyl 4-((S)-3-(benzyloxycarbonylamino)-2-oxopyrrolidin-1-yl)-3,3-dimethylpiperidine-1-carboxylate (0.81 g, 1.8 mmol, 23%) as a white solid.
WORKUP
后处理
- extractionextracted into ethyl acetate
- washThe organic layer was washed with 1 N HCl solution and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated under vacuum