反应详情

tert-Butyl(2R)-2-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-2-hydroxyethylcarbamate, (86.37 g) in DMF (600 ml) was added dropwise to a stirred suspension of sodium hydride (60% oil dispersion, 11.9 g) in DMF (160 ml) with cooling such that the internal temperature remained at 0° under nitrogen. The mixture was stirred at 21° for 2 h. The mixture was recooled to 0° and 2M HCl (134 ml) was added. The mixture was diluted with water and the product was extracted with EtOAc twice. The solution was washed with brine twice, dried (MgSO4) and evaporated to give the title compound (63.55 g). LCMS RT=2.66 min.

1. temperaturewith cooling such that the internal temperature
2. customremained at 0° under nitrogen
3. customwas recooled to 0°
4. extractionthe product was extracted with EtOAc twice
5. washThe solution was washed with brine twice
6. dry with materialdried (MgSO4)
7. customevaporated