反应详情

Into a 300 ml three-neck flask were added compound (E) (20.0 g, 0.061 mol), cuprous cyanide (6.3 g, 0.071 mol) and N,N-dimethylformamide (DMF) (63 ml). The mixture was agitated and refluxed for 6 hours while heating on a mantle heater. After completion of the reaction, the reaction mixture was cooled down to room temperature and a 28% aqueous ammonia (18 ml) was added, followed by agitating the mixture, adding n-heptane (50 ml) for extraction, filtering off an insoluble matter in the n-heptane layer, washing the layer with 6N-HCl (50 ml), further washing with water till the aqueous layer became neutral, concentrating under reduced pressure, recrystallizing the resulting raw crystals from ethanol (10 ml), filtering off and drying to obtain 4-(trans-4'-methyloxymethylcyclohexyl)benzonitrile (F) (6.4 g).

1. temperaturerefluxed for 6 hours
2. temperaturewhile heating on a mantle heater
3. customAfter completion of the reaction
4. stirringby agitating the mixture
5. extractionfor extraction
6. filtrationfiltering off an insoluble matter in the n-heptane layer
7. washwashing the layer with 6N-HCl (50 ml)
8. washfurther washing with water till the aqueous layer
9. concentrationconcentrating under reduced pressure
10. customrecrystallizing the resulting raw crystals from ethanol (10 ml)
11. filtrationfiltering off
12. customdrying