Micromolecular electrochemical probe and synthetic method and application thereof
A synthetic method and electrochemical technology, applied in the fields of biomedicine and life sciences, to achieve the effects of good stability, rapid and sensitive response, and excellent selectivity
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Embodiment 1
[0026] Embodiment 1: The synthetic route of small molecule electrochemical probe:
[0027] a. Add 3.5g of o-phenylenediamine, 13.0g of potassium thiocyanate, and 200mL of methanol into the container, and add bromine solution in methanol under the condition of a dry-ice acetone low-temperature bath. After the reaction is completed, stir at room temperature for 1.5h, suction filter, and filter Pour into 400mL of water, add 25mL of ammonia water to the filtrate after suction filtration, suction filtration, washing with water, and drying to obtain a yellow intermediate (I): 4,5-bis(isothiocyano)-1,2-o-phenylenediamine , its structural formula is as follows:
[0028]
[0029] The methanol solution of bromine is 3mLBr 2 Dissolve in 50mL methanol.
[0030] b. Weigh 3.0g of the above intermediate (I) and 5.5g of sodium sulfide, add 150mL of water, heat in an oil bath at 70°C for 0.5h, add 1.5mL of carbon disulfide in an ice-water bath, after the reaction is complete, heat in an o...
Embodiment 2
[0043] Embodiment 2: the chemical performance of small molecule electrochemical probe
[0044] Instruments and reagents
[0045] CHI832B electrochemical analyzer (Shanghai Chenhua Instrument Factory); all electrochemical experiments used a three-electrode system, with platinum wire as the auxiliary electrode, Ag / AgCl (saturated KCl) electrode as the reference electrode, and a bare gold electrode as the working electrode ( Diameter: 2.0mm). Differential pulse voltammetry experiments were performed in conventional electrochemical cells at room temperature. Before the experiment, the bare gold electrode was first immersed in a mixed solution of sulfuric acid and hydrogen peroxide (H 2 SO 4 :H 2 o 2 =7:3) Soak for 10-20min, then fully grind, then ultrasonically 1-2min with ethanol and double distilled water, and finally scan CV (0.1-0.5V) with 0.1mol / L sulfuric acid solution, repeat several times until When a stable CV image appears, take it out, wash it with distilled water...
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