反应详情

To [(S)-1-benzyloxymethyl-2-(2-iodo-1,1-diphenylethoxy)-ethyl]-carbamic acid tert-butyl ester (4.74 g, 8.07 mmol) in N,N-dimethylformamide (70 mL) at room temperature add sodium hydride (0.452 g, 11.3 mmol, 60% dispersion in mineral oil). Heat reaction mixture to 60° C. for 4 hours, cool to room temperature and dilute with ethyl acetate (˜400 mL). Wash with water and saturated aqueous sodium chloride, dry (magnesium sulfate), filter and concentrate. Purify on silica gel eluting with 0:100 to 20:80 ethyl acetate:hexanes to give the desired compound as an oil.

1. temperatureHeat
2. customreaction mixture to 60° C. for 4 hours
3. washWash with water and saturated aqueous sodium chloride
4. dry with materialdry (magnesium sulfate)
5. filtrationfilter
6. concentrationconcentrate
7. customPurify on silica gel eluting with 0:100 to 20:80 ethyl acetate