反应详情

温度

150 °C

Under N2, in a sealed tube, to 22 (19.7 mmol) in DMF 50 ml, 1-iodo-4-nitrobenzene (21.6 mmol), cesium carbonate (19.6 mmol), palladium acetate (0.98 mmol), copper bromide (0.2 mmol) and tributylphosphine (1.9 mmol) were added. The reaction was stirred at 150° C. overnight and, after cooling to room temperature, the mixture was extracted with ethyl acetate. The organic layer was then washed (3 times) with water, dried over Na2SO4 and the solvent removed via a rotary evaporator. The residue was purified by chromatography on silica gel using 9:1 hexane/ethyl acetate as the eluent to yield 4.62 g (81%) of 23 as a yellow solid.

1. temperatureafter cooling to room temperature
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was then washed (3 times) with water
4. dry with materialdried over Na2SO4
5. customthe solvent removed via a rotary evaporator
6. customThe residue was purified by chromatography on silica gel using 9:1 hexane/ethyl acetate as the eluent