反应详情

温度

80 °C

A stirred mixture of 4-iodoanisole (174.5 g.), 4'-bromo-3'-nitroacetophenone (162.5 g.) and copper powder (144 g.) was heated at 80°C. for 5 hours and the temperature was then gradually raised during 4 hours to 110°C. The stirred mixture was maintained at 110°C. for a further period of 3 days. The reaction mixture was cooled to room temperature and extracted with methylene dichloride. The extract was filtered and the filtrate evaporated under reduced pressure to remove methylene dichloride. The residue was distilled in vacuo to give the product, b.p. 200° - 210°C./0.6 mm., which solidified on cooling. This product was recrystallized from methanol to give 4-acetyl-4'-methoxy-2-nitrobiphenyl, m.p. 127° - 129°C. (novel intermediate A).

1. temperaturethe temperature was then gradually raised during 4 hours to 110°C
2. temperatureThe stirred mixture was maintained at 110°C. for a further period of 3 days
3. temperatureThe reaction mixture was cooled to room temperature
4. extractionextracted with methylene dichloride
5. filtrationThe extract was filtered
6. customthe filtrate evaporated under reduced pressure
7. customto remove methylene dichloride
8. distillationThe residue was distilled in vacuo
9. customto give the product, b.p. 200° - 210°C./0.6 mm
10. temperatureon cooling
11. customThis product was recrystallized from methanol