反应详情

温度

50 °C

10.4 g of sodium cyanide were dissolved in a mixture of 100 ml of dimethylformamide and 6 ml of water and initially charged. This solution was heated with stirring to 50° C., and 20.4 g of 2,5-dichloroindan-1-one, dissolved in 100 ml of dimethylformamide, were then added dropwise over a period of 60 minutes. After the addition had ended, stirring was continued at 50° C. for 1 hour. The mixture was then allowed to cool to room temperature and the solvent was stripped off using a rotary evaporator. The resulting crystal slurry was mixed with 200 ml of water and acidified to pH 4.5 using 10% by weight strength aqueous hydrochloric acid. The precipitated solid was filtered off with suction, washed with water, recrystallized from toluene and dried in a vacuum drying cabinet. This gave 18.5 g of 2-cyano-5-chloroindan-1-one (yield: 97% of theory).

1. additioninitially charged
2. temperatureThis solution was heated
3. additionwere then added dropwise over a period of 60 minutes
4. additionAfter the addition
5. stirringstirring
6. temperatureto cool to room temperature
7. customa rotary evaporator
8. additionThe resulting crystal slurry was mixed with 200 ml of water
9. filtrationThe precipitated solid was filtered off with suction
10. washwashed with water
11. customrecrystallized from toluene
12. customdried in a vacuum
13. customdrying cabinet