反应详情

In a 250 ml round-bottom flask fitted with reflux condenser, 4.9 g of p-t-butylbenzonitrile, 3.82 g of lithium chloride and 5.85 g of sodium azide and 8.2 g of triethylammonium bromide in 100 ml of DMF were heated at 120° C. for 8 hours. After cooling to room temperature, 100 ml of water were added and the mixture was admixed in an ice bath with dilute hydrochloric acid until no further precipitate was formed. The mixture was filtered with suction, the precipitate was washed with water and dried. Recrystallization from ethanol/water gave 4.4 g of colorless crystals.

1. customIn a 250 ml round-bottom flask fitted
2. temperaturewith reflux condenser
3. customwas formed
4. filtrationThe mixture was filtered with suction
5. washthe precipitate was washed with water
6. customdried
7. customRecrystallization from ethanol/water