反应详情

温度

70 °C

A mixture of 2-(4-bromomethylphenyl)benzonitrile (12 g) and potassium phtalimide (15 g) in DMF (200 ml) was stirred at 70° C. for 5 hours. After addition of water, the mixture was extracted with methylene chloride. The extract was washed with water, dried and concentrated to dryness to give crystals. Recrystallization from ethyl acetate-isopropyl ether gave colorless crystals. To a suspension of the crystals in methanol (500 ml) was added hydrazine hydrate (10 ml) and the mixture was refluxed for 12 hours. After evaporation of the solvent, the residue was dissolved in ethyl acetate and the solution was washed with IN-NaOH and water. The organic layer was dried and concentrated to dryness to give crystals (14.2 g, 93%).

1. extractionthe mixture was extracted with methylene chloride
2. washThe extract was washed with water
3. customdried
4. concentrationconcentrated to dryness
5. customto give crystals
6. customRecrystallization from ethyl acetate-isopropyl ether
7. customgave colorless crystals
8. temperaturethe mixture was refluxed for 12 hours
9. customAfter evaporation of the solvent
10. dissolutionthe residue was dissolved in ethyl acetate
11. washthe solution was washed with IN-NaOH and water
12. customThe organic layer was dried
13. concentrationconcentrated to dryness