反应详情

To a solution of (3S)-1-Cbz-3-(cyclohexylamino)pyrolidine (4.75 g, 15.1 mmol) and TEA (4.26 mL, 30.2 mmol) in DCM (50 mL) was added dropwise isobutyryl chloride (1.15 mL, 60.3 mmol). The reaction mixture was stirred at rt for 12 h and quenched with 1N HCl solution. The organic material was extracted with DCM (50 mL×2) followed by EtOAc (50 mL×2), and the extracts were washed with a saline, dried over MgSO4, and concentrated in vacuo. The residue was purified by column chomatography (EtOAc/Hex=1/3) to give the title compound (5.40 g, 96.7%).

1. customquenched with 1N HCl solution
2. extractionThe organic material was extracted with DCM (50 mL×2)
3. washthe extracts were washed with a saline
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chomatography (EtOAc/Hex=1/3)