A metal iridium complex that responds synergistically to tumor microenvironment ph/hypoxia and its application
A technology of metal iridium and complexes, which is applied in the field of phosphorescent metal iridium complexes, can solve the problems of reducing the effect and improving actual production, and achieves the effect of improving sensitivity and high signal-to-noise ratio
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Embodiment 1
[0034] The preparation of embodiment 1 probe Ir-NIR-pH-1
[0035] Synthesis of Compound 1-(benzo[b]thiophen-2-yl)-isoquinoline(Hiqbt)
[0036]
[0037]Under argon protection, 1-bromoisoquinoline (1g, 4.8mmol) and benzo[b]thiophen-2-ylboronic acid (856mg, 4.8mmol) were dissolved in tetrahydrofuran (24mL), and potassium carbonate solution ( 1M, 24mL) and tetrakistriphenylphosphine palladium (227mg, 0.24mmol, 5% n / n), react overnight at 60°C, and monitor the progress of the reaction with TCL. After the reaction was finished, cool to room temperature, reclaim the organic phase, extract the aqueous phase twice with dichloromethane and combine the organic phases, dry over anhydrous sodium sulfate, evaporate the solvent under reduced pressure, and separate by column chromatography to obtain a light yellow Hiqbt solid (85.6 %).
[0038] Synthesis of Compound 4-Ethynylphenol
[0039]
[0040] Trimethylsilylacetylene (1.9 mL, 13.44 mmol) was added dropwise to 4-iodophenol (2.04...
Embodiment 2
[0053] The synthesis of embodiment 2 probe Ir-NIR-1
[0054]
[0055] Take the synthesized iridium complex chlorine bridge dimer Ir 2 (iqbt) 4 Cl 2 (154mg, 0.1mmol), L2 (56mg, 0.2mmol) and a mixed solvent of dichloromethane and methanol (12mL, 2:1, volume ratio) were placed in a three-necked flask, and heated to reflux for 6h under an argon atmosphere. After the reaction, the reaction mixture was cooled to room temperature, and 1 mmol of ammonium hexafluorophosphate was added. The suspension was stirred for 15 min and filtered to remove insoluble inorganic salts. The solvent was evaporated under reduced pressure, and column chromatography gave dark red Ir-NIR-pH-1 solid (62%). 1 H NMR (400MHz, CD 3 CN-d 3 )δ9.07(d, J=8.4Hz, 3H), 8.57(dd, J=8.3, 1.4Hz, 1H), 8.43(s, 1H), 8.33(dd, J=5.0, 1.4Hz, 1H), 8.27(dd, J=5.1, 1.4Hz, 1H), 7.96–7.87(m, 6H), 7.87–7.79(m, 3H), 7.78–7.64(m, 3H), 7.49(d, J=6.9Hz, 3H), 7.36(dd, J=10.5, 6.6Hz, 2H), 7.22–7.10(m, 4H), 6.70(t, J=7.6Hz, 2H),...
Embodiment 3
[0056] Example 3 Determination of the absorption spectrum and phosphorescence spectrum of the probe Ir-NIR-pH-1.
[0057] Accurately weigh the probe Ir-NIR-pH-1 and the probe Ir-NIR-1, transfer them into 5mL volumetric flasks, dilute to volume with DMSO, and prepare a concentration of 1.0×10 -3 mol / L solution, pipette 25 μL of the solution into a 5mL volumetric flask, and use DMSO and PBS buffer solution with a pH of 7.4 to make a concentration of 1.0×10 -5 mol / L solution, so that the volume fraction of DMSO in the buffer solution is 10%, and its ultraviolet spectrum is measured. The phosphorescence spectrum was measured using the maximum absorption wavelength of the ultraviolet spectrum as the excitation wavelength of the phosphorescence spectrum. Accurately weigh the compound to be tested and prepare a concentration of 1.0×10 -5 The mol / L containing DMSO volume fraction is 10% PBS buffer solution, and its spectral properties under acidic and alkaline conditions are determi...
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