反应详情

Add benzyl bromide (75 mL, 630.55 mmol) to a suspension of potassium carbonate (85 g, 615.006 mmol) and (R)-4-[(1S,2S)-2-amino-3-(3,5-difluorophenyl)-1-hydroxypropyl]-2,2-dimethyloxazolidine-3-carboxylic acid tert-butyl ester (80 g, 207.25 mmol) in acetonitrile (900 mL). Heat to reflux for 16 hours, cool to room temperature, and dilute with ethyl acetate (2 L). Wash with ammonium chloride (1.5 L), saturated aqueous sodium chloride (1.5 L), dry (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 5:95 to 20:80 ethyl acetate:hexanes) to give the desired compound as a white solid (102.1 g, 87%).

1. temperatureHeat
2. temperatureto reflux for 16 hours
3. washWash with ammonium chloride (1.5 L), saturated aqueous sodium chloride (1.5 L)
4. dry with materialdry (magnesium sulfate)
5. filtrationfilter
6. concentrationconcentrate
7. custompurify
8. wash(silica gel chromatography, eluting with 5:95 to 20:80 ethyl acetate:hexanes)