A trinuclear copper alkynyl complex with amino acid recognition function and its preparation method
A technology for amino acids and complexes, applied in the field of amino acid recognition, can solve the problems of rare studies on complexes containing carbonyl groups in ligands, cumbersome pretreatment steps, etc.
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Embodiment 1
[0048] [Cu(CH 3 EN) 4 ](BF 4 )Synthesis:
[0049] 30.3 mmol Cu 2 O was dissolved in 40 mL of acetonitrile, to which 10 mL of HBF was slowly added dropwise 4 to red Cu 2 O completely disappeared, continued adding acetonitrile until the precipitation disappeared, suction filtration to remove unreacted solids, the solvent was removed under reduced pressure, and ether was added to obtain a white solid.
[0050] [Cu 2 (dppm) 2 (CH 3 EN) 4 ](BF 4 ) 2 Synthesis:
[0051] 8 mmol [Cu(CH 3 EN) 4 ](BF 4 ), 8 mmol of bis(diphenylphosphine)methane, and 40 mL of acetonitrile were added to the flask, and the reaction was carried out under nitrogen protection for 24 hours. Part of the solvent was removed, and ether was added as a white solid (yield 81%).
[0052] [Cu 3 (μ-dppm) 3 (μ 3 -η 1 -C≡CC 6 H 4 -C(O)H-4) 2 ](BF 4 )Synthesis:
[0053] To 0.12 mmol [Cu 2 (dppm) 2 (CH 3 EN) 4 ](BF 4 ) 2 , 0.15mmol of 4-trimethylsilylethynylbenzaldehyde was added with 0.24mmol...
Embodiment 2
[0057] [Cu(CH 3 EN) 4 ](BF 4 )Synthesis:
[0058] 30.3 mmol Cu 2 O was dissolved in 40 mL of acetonitrile, to which 10 mL of HBF was slowly added dropwise 4 to red Cu 2 O completely disappeared, continued adding acetonitrile until the precipitation disappeared, suction filtration to remove unreacted solids, the solvent was removed under reduced pressure, and ether was added to obtain a white solid.
[0059] [Cu 2 (dppm) 2 (CH 3 EN) 4 ](BF 4 ) 2 Synthesis:
[0060] 8 mmol [Cu(CH 3 EN) 4 ](BF 4 ), 8 mmol of bis(diphenylphosphine)methane, and 40 mL of acetonitrile were added to the flask, and the reaction was carried out under nitrogen protection for 24 hours. Part of the solvent was removed, and ether was added as a white solid (yield 81%).
[0061] [Cu 3 (μ-dppm) 3 (μ 3 -η 1 -C≡CC 6 H 4 -C(O)H-4) 2 ](BF 4 )Synthesis:
[0062] To 0.12 mmol [Cu 2 (dppm) 2 (CH 3 EN) 4 ](BF 4 ) 2 , 0.15mmol of 4-trimethylsilylethynylbenzaldehyde was added with 0.24mmol...
Embodiment 3
[0066] UV-Vis absorption spectroscopy titration detection:
[0067] Take the [Cu] prepared in Example 1 3 (μ-dppm) 3 (μ 3 -η 1 -C≡CC 6 H 4 -C(O)H-4) 2 ](BF 4 ) 10μmol / L, and add cysteine, carry out UV-Vis absorption spectrum titration, the results are as follows Figure 4 As shown, it can be concluded that the binding constant of the trinuclear copper alkynyl complex prepared in Example 1 to cysteine is IgK=4.41±0.05.
[0068] Take the [Cu] prepared in Example 1 3 (μ-dppm) 3 (μ 3 -η 1 -C≡CC 6 H 4 -C(O)H-4) 2 ](BF 4 ) 10μmol / L, and added homocysteine, and titrated by UV-Vis absorption spectrum. The results are as follows Figure 5 As shown, it can be concluded that the binding constant of the trinuclear copper alkynyl complex prepared in Example 1 and homocysteine is lgK=4.84±0.11.
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