反应详情

2,3-Dicyano-5-chloro-6-phenylpyrazine (12.03 g; 0.05 mole) was dissolved in 1,400 ml of toluene. The solution was cooled to 5° to 10° C., and with stirring, 3.25 g (0.055 mole) of n-propylamine was added dropwise over the period of 10 minutes. Subsequently, 55 ml of a 1 N aqueous solution of sodium hydroxide was added dropwise over the period of 10 minutes. The mixture was then stirred at 5° to 10° C. for 30 minutes. After the reaction, the reaction mixture was separated into two layers. The toluene layer was concentrated under reduced pressure to obtain a solid. The solid was washed twice with 200 ml of water, dried under reduced pressure, and recrystallized successively from toluene and ethanol to afford 12.1 g (yield 92%) of 2,3-dicyano-5-n-propylamino-6-phenylpyrazine.

1. temperatureThe solution was cooled to 5° to 10° C.
2. stirringThe mixture was then stirred at 5° to 10° C. for 30 minutes
3. customAfter the reaction
4. customthe reaction mixture was separated into two layers
5. concentrationThe toluene layer was concentrated under reduced pressure
6. customto obtain a solid
7. washThe solid was washed twice with 200 ml of water
8. customdried under reduced pressure
9. customrecrystallized successively from toluene and ethanol