反应详情

To a solution of 5-tert-butoxycarbonylamino-2-hydroxybenzoic acid (1.02 g, 4.02 mmole) in DMF (20.0 ml) was added with acetyl chloride (39 mg, 4.83 mmole) and potassium carbonate (555 mg, 4.02 mmole). The reaction mixture was stirred for 4 hr at room temperature. After the reaction mixture was concentrated, the residue was dissolved in ethyl acetate. The organic layer was washed with water and brine and dried over anhydrous Na2SO4. After evaporation of the solvent, the residue was recrystallized from ethyl acetate/hexane to give 0.62 g (52% yield) of 2-ethanoyloxy-5-tert-butoxycarbonylaminobenzoic acid as a white solid.

1. concentrationAfter the reaction mixture was concentrated
2. dissolutionthe residue was dissolved in ethyl acetate
3. washThe organic layer was washed with water and brine
4. dry with materialdried over anhydrous Na2SO4
5. customAfter evaporation of the solvent
6. customthe residue was recrystallized from ethyl acetate/hexane