反应详情

Add 68.6 ml (663 mmol) diethylamine dropwise to a mixture of 60.0 g (301 mmol) bromoacetophenone and 25.89 g (391.86 mmol) malononitrile in 130 ml DMF at RT (cooling is required to maintain the temperature). Towards the end of addition, remove the cooling, stir the mixture for 1 h at RT and then add water to 385 ml. Dilute with a further 125 ml water and stir for 20 min at RT. Filter off the precipitated solids with suction, wash twice with 125 ml water each time, dry under suction and wash with petroleum ether. Dry the residue at high vacuum. 33.3 g (50.1% of theor.) of the target compound is obtained as yellowish-brown crystals.

1. temperaturecooling
2. temperatureto maintain the temperature)
3. additionTowards the end of addition
4. customremove the cooling
5. additionDilute with a further 125 ml water
6. stirringstir for 20 min at RT
7. filtrationFilter off the precipitated solids with suction
8. washwash twice with 125 ml water each time
9. customdry under suction
10. washwash with petroleum ether
11. customDry the residue at high vacuum
12. custom33.3 g (50.1% of theor.) of the target compound is obtained as yellowish-brown crystals