反应详情

温度

60 °C

To a solution of (4R)-1-(tert-butoxy carbonyl)-4-hydroxy-L-proline in DMF (80 ml) was added 5.4 g of NaHCO3 and 11.1 g of benzyl bromide and the reaction mixture was stirred at 60° C. for 5 hours. Water was added to the reaction solution and the resulting mixture was extracted with EtOAc. The extract was dried over Na2SO4, then, the drying agent was separated by filtration and the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography (silicagel 60; mobile phase: hexane/EtOAc=1/1 to CHCl3/MeOH=8/1; v/v) to obtain 10.0 g of the title compound (colorless oil).

1. extractionthe resulting mixture was extracted with EtOAc
2. dry with materialThe extract was dried over Na2SO4
3. customthe drying agent was separated by filtration
4. customthe solvent was evaporated under reduced pressure
5. customThe obtained residue was purified by column chromatography (silicagel 60; mobile phase: hexane/EtOAc=1/1 to CHCl3/MeOH=8/1; v/v)