反应详情

温度

110 °C

A suspension of methyl 3-(acetylamino)-6-bromo-2-nitrobenzoate (500 mg, 1.58 mmol), palladium acetate (36.0 mg, 0.16 mmol), triphenylphosphine (84.0 mg, 0.32 mmol), potassium carbonate (328 mg, 2.37 mmol) and methyl acrylate (213 μL, 2.37 mmol) in N,N-dimethylformamide (15 mL) was stirred under a nitrogen atmosphere at 110° C. for 30 min with heating. The reaction solution was diluted with water, extracted with ethyl acetate, washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=25/75→55/45) to give the title compound (303 mg, yield 60%).

1. temperaturewith heating
2. extractionextracted with ethyl acetate
3. washwashed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane=25/75→55/45)