反应详情

温度

60 °C

A mixture of 4-nitro-phthalonitrile (1 eq), 2,6-dimethylphenol (1.2 eq), K2CO3 (2 eq), and DMF (1 mL/mmol 4-nitro-phthalonitrile) was heated under nitrogen at 60° C. for 3 h with stirring After cooling to ambient temperature the mixture was poured into water (6 mL/mL DMF) with stirring. The mixture was extracted twice with EtOAc. The combined organic phases were dried over MgSO4 and concentrated in vacuo. The residue was recrystallized from EtOH to give the title compound as a tan solid (yield: 87%); 1H NMR (CDCl3, 200 MHz): δ=7.70 (d, 1H), 7.05 to 7.16 (m, 5H), 2.08 (s, 6H).

1. temperatureAfter cooling to ambient temperature the mixture
2. stirringwith stirring
3. extractionThe mixture was extracted twice with EtOAc
4. dry with materialThe combined organic phases were dried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was recrystallized from EtOH