反应详情

温度

42.5 °C

To a suspension of 6.60 g (33.7 mmol) of (2R, 4R)-(+)-2-(ethoxycarbonyl)-4-hydroxypyrrolidine hydrochloride in acetonitrile (60 ml) were added 8.22 g (77.6 mmol) of sodium carbonate, 4-methoxyphenethyl bromide (8.71 g, 40.5 mmol), and sodium iodide (150mg, 1.0 mmol) and the mixture was stirred at 40-45° C. for 65 h. The mixture was concentrated in vacuo and water was added to the residue, and the products were extracted with ethyl acetate. The extract was washed with saturated aqueous sodium chloride and the products were extracted with 10% aqueous hydrochloride. The extract was washed with ethyl acetate, basified with potassium carbonate and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, dried over anhydrous sodium sulfate, and concentrated in vacuo to obtain oily (2R, 4R)-(+)-2-(ethoxycarbonyl)-4-hydroxy-1-(4-methoxy phenethyl) pyrrolidine (5.85 g, 59.1%).

1. concentrationThe mixture was concentrated in vacuo and water
2. additionwas added to the residue
3. extractionthe products were extracted with ethyl acetate
4. washThe extract was washed with saturated aqueous sodium chloride
5. extractionthe products were extracted with 10% aqueous hydrochloride
6. washThe extract was washed with ethyl acetate
7. extractionextracted with ethyl acetate
8. washThe organic layer was washed with saturated aqueous sodium chloride
9. dry with materialdried over anhydrous sodium sulfate
10. concentrationconcentrated in vacuo