Aluminum ion fluorescent probe and preparation method thereof
A technology of fluorescent probes and aluminum ions, applied in the field of fluorescent probes, can solve the problems of complex operation process, long detection time, high requirements for instruments, etc., and achieve the effect of good selectivity
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Embodiment 1
[0040] A preparation method for an aluminum ion fluorescent probe, comprising the following steps:
[0041] Step 1: Add 10g of hexamethylenetetramine and 5g of 7-hydroxycoumarin to a clean 250mL round-bottomed flask in sequence, then add 50mL of glacial acetic acid, stir the reactants well, adjust the reaction temperature to 95°C and heat Reflux for 5 hours, then transfer 75 mL of prepared hydrochloric acid with a mass concentration of 20% to the reactant, adjust the temperature to 60°C and heat for 30 minutes, then place the reactant to cool, and extract the reacted liquid with the organic solvent diethyl ether (50mL×3), combined the extracted organic matter, then added anhydrous MgSO 4 Carry out drying, the organic matter after drying is concentrated and obtain crude product, finally with dehydrated alcohol, crude product recrystallization, obtains 1.25g pale yellow strip solid, i.e. 7-hydroxycoumarin-8-aldehyde, productive rate is 21 %.
[0042] The NMR characterization d...
Embodiment 2
[0046] A preparation method for an aluminum ion fluorescent probe, comprising the following steps:
[0047] Step 1: Add 5g of hexamethylenetetramine and 5g of 7-hydroxycoumarin to a clean 250mL round-bottomed flask in turn, then add 50mL of glacial acetic acid, stir the reactants well, adjust the reaction temperature to 95°C and heat Reflux for 4 hours, then transfer 75 mL of prepared hydrochloric acid with a mass concentration of 20% to the reactant, adjust the temperature to 40°C and heat for about 50 minutes, then place the reactant to cool, and extract the reacted substance with diethyl ether, an organic solvent. liquid (50mL×3), combined the extracted organic matter, then added anhydrous MgSO 4 Carry out drying, the organic matter after drying is concentrated and obtain crude product, finally use dehydrated alcohol to crude product recrystallization, thereby obtain 0.65g pale yellow strip solid, i.e. 7-hydroxycoumarin-8-aldehyde, productive rate is 11%.
[0048] Step 2,...
Embodiment 3
[0050] A preparation method for an aluminum ion fluorescent probe, comprising the following steps:
[0051] Step 1: Add 7.5g of hexamethylenetetramine and 5g of 7-hydroxycoumarin to a clean 250mL round-bottomed flask in sequence, then add 50mL of glacial acetic acid, stir the reactants thoroughly, and adjust the reaction temperature to 95°C Heat to reflux for 6h, then transfer 75mL of prepared hydrochloric acid with a mass concentration of 20% to the reactant, adjust the temperature to 80°C and heat for about 20min, then place the reactant to cool, and extract the reactant with an organic solvent ether liquid (50mL×3), combined the extracted organic matter, then added anhydrous MgSO 4 Carry out drying, the organic matter after drying is concentrated and obtain crude product, finally use absolute ethanol to crude product recrystallization, thereby obtain 0.91g pale yellow strip solid, i.e. 7-hydroxycoumarin-8-aldehyde, productive rate is 16%.
[0052] Step 2, first add 0.38g ...
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