反应详情

温度

60 °C

A mixture of 4-nitrophthalonitrile (10.6 g, 60.0 mmol), o-cresol (7.9 g, 72.0 mmol) and K2CO3 (16.6 g, 120.0 mmol) in DMF (70 mL) was heated to 60° C. under a nitrogen atmosphere for 3 hours. The crude reaction was then poured into H2O (300 mL). The resulting mixture was extracted twice with EtOAc. The combined organic layers were washed with sat'd NaHCO3 solution, dried over MgSO4 and concentrated in vacuo. The residue was then dissolved in EtOH (60 mL). After storing for 5 hours at room temperature, the precipitate was collected by filtration and the filter cake was washed with cold EtOH to give the title compound in 8.9 g. MS: (+) m/z 235.46 (M+1).

1. customThe crude reaction
2. extractionThe resulting mixture was extracted twice with EtOAc
3. washThe combined organic layers were washed with sat'd NaHCO3 solution
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. dissolutionThe residue was then dissolved in EtOH (60 mL)
7. filtrationthe precipitate was collected by filtration
8. washthe filter cake was washed with cold EtOH