Preparation method of 1-(acetyl bromide)pyrene

[0016] Example 1

[0017] At room temperature, in a 5L four-necked reaction flask equipped with mechanical stirring, add 115.4g pyrene, 1.8L dichloromethane, 1.73g tetrabutylammonium bromide and 5.19g tetraethylammonium bromide. Put it in an ice-salt bath to control the temperature at -5℃~0℃ and stir until it is completely dissolved; add 115g bromoacetyl bromide at one time, the solution becomes brownish black after stirring; then add 87.4g anhydrous aluminum trichloride and 1.2L Dichloromethane, stir, the color of the solution turns purple and black, and gradually viscous, keep the above temperature and stir for 4 hours, after the reaction, slowly pour the reaction solution into 10kg of crushed ice to quench, then adjust with 10% sodium bicarbonate solution PH≈8, separate and collect the organic phase, wash the organic phase with water for 2 to 3 times, spin-dry the solvent with a rotary evaporator, and collect the solid to be the crude product. The crude product is dissolved in dichloromethane, decolorized by adding activated carbon, filtered, and then recrystallized once with a mixture solvent of dichloromethane and petroleum ether in a volume ratio of 2:1, and a bright yellow product is obtained after drying.

[0018] Example 2

[0019] At room temperature, in a 5L four-necked reaction flask equipped with mechanical stirring, add 101.1g pyrene, 1.5L dichloromethane, 1.44g tetrabutylammonium bromide and 4.33g tetraethylammonium bromide respectively, and place the reaction flask Put it in an ice-salt bath and stir at -5℃~0℃ to dissolve it completely; add 100.1g bromoacetyl bromide at one time, and the solution will be brown and black after stirring; then add 76.1g anhydrous aluminum trichloride and 1 L Dichloromethane, stir, the color of the solution turns purple and black, and gradually viscous, keep the above temperature and stir for 4.5 hours, after the reaction, slowly pour the reaction solution into 10kg of crushed ice to quench, and then adjust with 10% sodium bicarbonate solution PH≈8, separate and collect the organic phase, wash the organic phase with water for 2 to 3 times, spin-dry the solvent with a rotary evaporator, and collect the solid to be the crude product. The crude product is dissolved in dichloromethane, decolorized by adding activated carbon, filtered, and then recrystallized once with a mixture solvent of dichloromethane and petroleum ether in a volume ratio of 2:1, and a bright yellow product is obtained after drying.

[0020] Example 3

[0021] At room temperature, in a 5L four-necked reaction flask equipped with mechanical stirring, add 121.4g pyrene, 2.1L dichloromethane, 1.97g tetrabutylammonium bromide and 5.90g tetraethylammonium bromide respectively, and place the reaction flask Put it in an ice-salt bath and stir at -5℃~0℃ to dissolve it completely; add 121.1g bromoacetyl bromide at one time, and the solution will be brown-black after stirring; then add 76.1g anhydrous aluminum trichloride and 1.4 L Dichloromethane, stir, the color of the solution turns purple and black, and gradually viscous, keep the above temperature and stir for 4.5 hours, after the reaction, slowly pour the reaction solution into 10kg of crushed ice to quench, and then adjust with 10% sodium bicarbonate solution PH≈8, separate and collect the organic phase, wash the organic phase with water for 2 to 3 times, spin-dry the solvent with a rotary evaporator, and collect the solid to be the crude product. The crude product is dissolved in dichloromethane, decolorized by adding activated carbon, filtered, and then recrystallized once with a mixture solvent of dichloromethane and petroleum ether in a volume ratio of 2:1, and a bright yellow product is obtained after drying.