Preparation method of fluorescent ketone reagent
A technology of fluorescent ketones and reagents, which is applied in the field of preparation of fluorescent ketone reagents, can solve the problems of limiting the application of fluorescent reagents, difficult to handle toxic gases, and long reaction time, so as to shorten the heat conduction time, optimize the reaction sequence, and temperature easy to control effects
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[0030] A preparation method for fluorone reagents, comprising the following steps:
[0031] Accurately measure 4.6g of resorcinol and 2.3mL of benzaldehyde in a 250mL flat-bottomed flask, add catalysts of different mass ratios (the amount of catalyst p-toluenesulfonic acid is 1-2% of the mass of the reactant), connect the reflux device and insert In the microwave reactor, set the time and power. After the reaction is complete, move the product into a large beaker, add a sodium hydroxide solution with a mass fraction of 10%, wash with alkali until the pH value is about 12, add concentrated hydrochloric acid drop by drop, adjust When the pH value reaches about 3, filter under reduced pressure and wash with deionized water until the pH reaches 6. Dry, weigh, and recrystallize three times with acetone or ethanol. Multiple experiments were conducted to explore anyway the optimal catalyst dosage, time and microwave power.
[0032] The microwave heater power is 195-325W.
[0033] ...
Embodiment 1
[0035] Accurately measure 4.6g of resorcinol and 2.3mL of benzaldehyde into a 250mL flat-bottomed flask, and add different mass ratios of catalyst p-toluenesulfonic acid. Connect the reflux device and plug into the microwave reactor, set the time and power. After the reaction is complete, move the product into a large beaker, add a 10% sodium hydroxide solution, wash with alkali until the pH value is about 12, add concentrated hydrochloric acid drop by drop, adjust the pH value to about 3, filter under reduced pressure, and remove Wash with deionized water until the pH is around 6. Dry and weigh. The crude product is dissolved and recrystallized three times with acetone or ethanol, which is a fluorescent ketone reagent. Multiple experiments explored the optimal catalyst dosage, time and microwave power for the reaction.
[0036] figure 1 It is a reaction flow diagram of the present invention.
[0037] Under the premise of fixing the initial feed ratio (the mass volume rat...
Embodiment 2
[0045] Traditional method:
[0046] Get 4.6g (0.04mol) resorcinol, 0.069g p-toluenesulfonic acid (consumption is 1.5% of reactant mass) in the there-necked flask, add 2.2mL benzaldehyde dropwise thereinto, control reaction temperature to be 100-120 ℃, stirring the reaction for 2h. Add a NaOH solution with a mass fraction of 5% to the reaction solution until the product is completely dissolved, adjust the pH of the system to 3 with hydrochloric acid, and suction filter to obtain a solid after standing for 1 h, add deionized water to wash the precipitate until the pH of the filtrate is 7, and the solid Place in an oven to dry for 8h, using ethanol-water (V 乙醇 :V 去离子水=1:4) recrystallized, centrifuged to obtain orange microcrystalline powder, and dried at 70°C for 8 hours to obtain fluorone reagents with a yield of 26% and a purity of 87%.
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