反应详情

In 15 ml of DMF were dissolved 2.8 g of N-t-butoxycarbonyl-(S)-proline and 2.8 g of phenylcarbamoyl methyl bromide. To the solution was added 1.1 g of sodium hydrogencarbonate. The mixture was stirred at room temperature for 20 hours. The reaction mixture was poured into ice water, followed by extraction with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium hydrogencarbonate and with water and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (using chloroform as an eluent), giving the title compound as a colorless oil. Yield 3.5 g.

1. extractionfollowed by extraction with ethyl acetate
2. washThe extract was washed with a saturated aqueous solution of sodium hydrogencarbonate and with water
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvent was distilled off under reduced pressure
5. customthe residue was purified by silica gel column chromatography (