反应详情

温度

115 °C

To a flask (100 mL) with magnetic stirrer was added 6-methoxy-1H-benzo[d][1,3]oxazine-2,4-dione (1.55 g, 8.00 mmol), 4-sec-butylaniline (1.19 mL, 8.0 mmol) and anhydrous DMF (10 mL). The reaction mixture was stirred at 115° C. for 16 hours under nitrogen. DMF was removed and the residue was mixed with water (100 mL) and ethyl acetate (150 mL). The organic phase was separated and washed with brine (50 mL). The solvent was removed and the residue was purified by column chromatography on silica gel (230-400 mesh) using hexane/ethyl acetate=1:1 to give 2-amino-N-(4-sec-butyl-phenyl)-5-methoxy-benzamide. Yield: 0.90 g (37%).

1. customDMF was removed
2. additionthe residue was mixed with water (100 mL) and ethyl acetate (150 mL)
3. customThe organic phase was separated
4. washwashed with brine (50 mL)
5. customThe solvent was removed
6. customthe residue was purified by column chromatography on silica gel (230-400 mesh)