A kind of 1,10-phenanthroline derivative and its preparation method and application
A technology of phenanthroline and derivatives, applied in the field of 1,10-phenanthroline derivatives, can solve the problems of high synthesis difficulty and complex ligand structure, and achieve the effects of high selectivity, pH stability and low cost
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Embodiment 1
[0021] Step 1. Add 2.12 g (87.4 mmol) activated magnesium chips, 10 mL anhydrous tetrahydrofuran and 0.02 g catalytic amount of iodine to a 100 mL dry three-necked flask, and stir slowly at room temperature under the protection of argon; 7.85 mL 4-Bromopropoxybenzene (62.5 mmol) was dissolved in 10 mL of anhydrous tetrahydrofuran to make a solution, and slowly added dropwise to the above-mentioned three-necked flask, keeping the reaction system at a slight boil, after the drop, heated to reflux for 30 minutes Cool to room temperature to make Grignard reagent.
[0022] Step 2. Add 7.82 g (23.1 mmol) 3,8-dibromo-1,10-phenanthroline, 0.34 g (0.64 mmol) [Ni(dppp )Cl 2 ] catalyst and 80 mL of anhydrous tetrahydrofuran, pour the reaction solution in step 1 into a 50 mL dropping funnel, then slowly drop it into the above-mentioned three-necked bottle, stir at room temperature for 2 hours after dropping, and then heat to reflux for 12 hours, cooled to room temperature. Quenched by ...
Embodiment 2
[0025] Step 1 and step 2 are the same as in Embodiment 1.
[0026] Step 3: Compounding 3,8-bis(4-propoxyphenyl)-1,10-phenanthroline into 10 -4 mol / L solution, its fluorescence titration spectrum in ethanol-water solution is as follows image 3 As shown, with Zn 2+ content increases, the fluorescence emission intensity of the solution at 461 nm increases linearly, when Zn 2+ When the content reaches 1.2 equivalents, the fluorescence intensity reaches the maximum value. The fluorescence peak of the ligand is at 402 nm. Compared with the ligand, the emission spectrum of the complex is red-shifted by 59 nm. Competition experiments with different metal ions such as Figure 4 As shown, alkali metal ions, alkaline earth metal ions and some transition metal ions do not cause great interference. Figure 5 It is the Job curve, indicating that the ligand and the zinc ion present a 1:1 complex form in solution, which is consistent with figure 2 The crystal structure data agree wel...
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