反应详情

To a solution of 4-bromo-2-methylaniline (1 g, 5.37 mmol,) in 1,4-dioxane (11 mL) and H2O (4 mL), at r.t., were added Et3N (2.7 mL, 1.2 eq) and BOC2O (4.2 g, 1.2 eq). The reaction mixture was stirred at r.t. for 96 hr. Sat.aq. NH4Cl and EtOAc (20 mL) were added and the phases were separated. The aqueous layer was further extracted with EtOAc (2×20 mL). The combined organic extracts were dried over anh. Na2SO4, the solids were filtered and the solvent evaporated. The residue was purified on an SCX cartridge (CH2Cl2, MeOH and NH3(0.5 M in MeOH)) to give the title compound as a white solid (1.22 g, 79%).

1. customthe phases were separated
2. extractionThe aqueous layer was further extracted with EtOAc (2×20 mL)
3. dry with materialThe combined organic extracts were dried over anh. Na2SO4
4. filtrationthe solids were filtered
5. customthe solvent evaporated
6. customThe residue was purified on an SCX cartridge (CH2Cl2, MeOH and NH3(0.5 M in MeOH))