HRID408022

反应详情

EQUATION

反应方程式

HRID 408022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. extractionextracted into ethyl acetate
  2. washThe organic layer was washed with 1 N HCl solution and brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum