反应详情

温度

100 °C

To the mixture of (3S)-1-Cbz-3-(cyclohexylamino)pyrrolidine (3.0 g, 10 mmol), TEA (15 mL), and DMAP (1.25 g, 10 mmol) in THF (15 mL) was added 2,2-dimethyl-3-acetyloxypropionyl chloride (3.58 g, 20 mmol) prepared in Step A. After the reaction mixture was refluxed for 48 h (90-110° C.), the solvent was removed, and the residue was diluted with an aqueous NaHCO3 solution was added to the residue. The organic material was extracted with EtOAc, and the extracts were washed by 1N HCl, dried over MgSO4, and concentrated in vacuo. The crude product was purified by column chomatography (EtOAc/Hex=1/2) to give the title compound (2.80 g, 62.9%).

1. customthe solvent was removed
2. additionthe residue was diluted with an aqueous NaHCO3 solution
3. additionwas added to the residue
4. extractionThe organic material was extracted with EtOAc
5. washthe extracts were washed by 1N HCl
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by column chomatography (EtOAc/Hex=1/2)