反应详情

温度

110 °C

An anhydrous toluene (40 mL) suspension of 1-nitronaphthalen-2-yl triflate (3.00 g, 8.64 mmol), 3-aminobenzonitrile (1.02 g, 8.64 mmol), potassium carbonate (1.19 g, 8.64 mmol), triphenylphosphine (227 mg, 0.864 mmol), and tetrakis(triphenylphosphine)palladium (500 mg, 0.432 mmol) was stirred at 110° C. for 18 hours. After cooling on standing, the reaction mixture was filtered, and the filtrate was diluted with ethyl acetate. The obtained organic solution was washed with a saturated aqueous sodium hydrogen carbonate solution, and dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure, and the residue was purified by silica gel column chromatography (chloroform/methanol=99/1) to obtain the titled compound as a yellow powder (1.60 g, yield 64%).

1. temperatureAfter cooling
2. filtrationthe reaction mixture was filtered
3. additionthe filtrate was diluted with ethyl acetate
4. washThe obtained organic solution was washed with a saturated aqueous sodium hydrogen carbonate solution
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent was removed by evaporation under reduced pressure
7. customthe residue was purified by silica gel column chromatography (chloroform/methanol=99/1)