Method for synthesizing 2-acetyl-1, 10-phenanthroline (3)

[0024] The method for preparing 2-acetyl-1,10-phenanthroline (3), comprising adding 1,10-phenanthroline and dichloroethane to a container at a mass ratio of 1:50, and then placing the container in an ice-water bath Under stirring, and add trifluoromethanesulfonic anhydride, the mass ratio of the addition amount of trifluoromethanesulfonic anhydride and 1,10-phenanthroline is 1:1, then the container is placed at room temperature and stirred for 1 hour, and trimethylsulfonic acid is added Cyanosilane, the mass ratio of trimethylsilyl cyanide to 1,10-phenanthroline is 4:1, then the container is heated to 84°C, and stirring is continued for 4 hours, and finally 1,8-diazepine is added Dicycloundec-7-ene (DBU), the mass ratio of 1,8-diazabicycloundec-7-ene (DBU) to 1,10-phenanthroline is 0.5:1 , stirred at 84°C for 17 hours, cooled the mixture to room temperature, quenched with saturated sodium bicarbonate solution, extracted with dichloromethane, washed with saturated sodium chlori...

[0026] Referring to Example 1, the method for preparing 2-acetyl-1,10-phenanthroline (3) includes adding 1,10-phenanthroline and dichloroethane to the container at a mass ratio of 1:100, and then The container was placed in an ice-water bath and stirred, and trifluoromethanesulfonic anhydride was added, and the mass ratio of the amount of trifluoromethanesulfonic anhydride to 1,10-phenanthroline was 1: 4, and then the container was stirred at room temperature for 1 hour, add trimethylsilyl cyanide, the mass ratio of the amount of trimethylsilyl cyanide to 1,10-phenanthroline is 2:1, then the container is warmed up to 84 ° C, continue to stir for 4 hours, and finally add 1, The amount of 8-diazabicycloundec-7-ene (DBU), 1,8-diazabicycloundec-7-ene (DBU) and the quality of 1,10-phenanthroline The ratio is 3:1, stirred at 84°C for 17 hours, cooled the mixture to room temperature, quenched with saturated sodium bicarbonate solution, extracted with dichloromethane, washed with satu...

[0028]Reference Example 1, the method for preparing 2-acetyl-1, 10-, phenanthroline (3), including adding 1, 10-phenanthroline and dichloroethane to the container at a mass ratio of 1:75, and then Place the container under an ice-water bath for stirring, and add trifluoromethanesulfonic anhydride, the mass ratio of the amount of trifluoromethanesulfonic anhydride to 1,10-phenanthroline is 1:2, and then place the container at room temperature to stir For 1 hour, add trimethylsilyl cyanide, the mass ratio of the amount of trimethylsilyl cyanide to 1,10-phenanthroline is 5:1, then the container is heated to 84°C, and stirring is continued for 4 hours, and finally 1 , 8-diazabicycloundec-7-ene (DBU), the amount of 1,8-diazabicycloundec-7-ene (DBU) and 1,10-phenanthroline The mass ratio is 2:1, stirred at 84°C for 17 hours, cooled the mixture to room temperature, quenched with saturated sodium bicarbonate solution, extracted with dichloromethane, washed with saturated sodium chlori...