反应详情

温度

55 °C

60 g of KOH are dissolved in 300 ml of methanol and heated up to 55° C. To the solution are added 32.2 g (0.27 mol) of phenylacetonitrile followed by 30.8 g (0.25 mol) of nitrobenzene. The reaction mixture is stirred at 55° C. for 4 hrs. After cooling, 400 ml of water are added with stirring. The resulting solution is acidified by addition of 110 ml of acetic acid in 100 ml of water, leading to a yellow-orange precipitate. The mixture is then filtered, and the yellow solid is washed with a mixture of methanol and water. The crude product is dried in air, boiled with 150 ml of benzene for 15 min., cooled, filtered and dried under vacuum. 42.6 g (77%) of (4-Hydroxyimino-cyclohexa-2,5-dienylidene)-phenyl-acetonitrile are obtained in the form of a yellow solid having a melting point of 159-163° C. (dec.).

1. temperatureAfter cooling
2. stirringwith stirring
3. filtrationThe mixture is then filtered
4. washthe yellow solid is washed with a mixture of methanol and water
5. dry with materialThe crude product is dried in air
6. waitboiled with 150 ml of benzene for 15 min.
7. temperaturecooled
8. filtrationfiltered
9. customdried under vacuum