Preparation method of 1-(acetyl bromide)pyrene
A technology of bromoacetyl and bromoacetyl bromide, which is applied in the field of preparation of 1-(bromoacetyl)pyrene, can solve the problems of high price, increased energy consumption, and high production cost, and achieves production cost reduction, color improvement, and simple operation Effect
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Embodiment 1
[0017] At room temperature, in a 5L four-necked reaction flask equipped with mechanical stirring, add 115.4g of pyrene, 1.8L of dichloromethane, 1.73g of tetrabutylammonium bromide and 5.19g of tetraethylammonium bromide respectively, and the reaction flask Put it into an ice-salt bath with temperature control -5°C to 0°C and stir until it is completely dissolved; add 115g of bromoacetyl bromide at one time, stir evenly and the solution turns brownish black; then add 87.4g of anhydrous aluminum trichloride and 1.2L of Dichloromethane, stirring, the color of the solution turns purple and black, and gradually viscous. Keep the above temperature and stir for 4 hours. After the reaction is completed, the reaction solution is slowly poured into 10kg of crushed ice to quench, and then adjusted with 10% sodium bicarbonate solution. PH≈8, separate the liquid to collect the organic phase, wash the organic phase with water for 2 to 3 times, spin dry the solvent with a rotary evaporator, ...
Embodiment 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, put the reaction flask Put it into an ice-salt bath and control the temperature at -5°C to 0°C and stir until it is completely dissolved; add 100.1g of bromoacetyl bromide at one time, stir evenly, and the solution turns brownish black; then add 76.1g of anhydrous aluminum trichloride and 1 L of Dichloromethane, stirring, the solution color turns purple black, and gradually viscous, keep the above temperature stirring reaction for 4.5 hours, after the reaction is completed, the reaction solution is slowly poured into 10kg of crushed ice to quench, and then adjusted with 10% sodium bicarbonate solution PH≈8, separate the liquid to collect the organic phase, wash the organic phase with water for 2 to 3 times, spin dry the solvent with a rotary evaporator, and c...
Embodiment 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, put the reaction flask Put it into an ice-salt bath and control the temperature at -5°C to 0°C and stir until it is completely dissolved; add 121.1g of bromoacetyl bromide at one time, stir evenly, and the solution turns brownish black; then add 76.1g of anhydrous aluminum trichloride and 1.4 L of Dichloromethane, stirring, the solution color turns purple black, and gradually viscous, keep the above temperature stirring reaction for 4.5 hours, after the reaction is completed, the reaction solution is slowly poured into 10kg of crushed ice to quench, and then adjusted with 10% sodium bicarbonate solution PH≈8, separate the liquid to collect the organic phase, wash the organic phase with water for 2 to 3 times, spin dry the solvent with a rotary evaporator, and...
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