A fluorescent probe capable of simultaneously detecting β-amyloid deposition plaques and peroxynitrite, its preparation method and application
A technology of peroxynitrite and amyloid, applied in chemical instruments and methods, fluorescence/phosphorescence, material analysis through optical means, etc., can solve the problem of few small molecule fluorescent probes, achieve good staining effect, The effect is simple and easy to promote
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[0052] The preparation method of above-mentioned fluorescent probe, comprises the steps:
[0053] The reaction equation is:
[0054]
[0055] 1) dissolving compound 1 in glacial acetic acid, and adding diethyl ketomalonate therein and stirring evenly to obtain a mixed solution;
[0056] 2) After reacting the mixed solution in 1) for a set time and temperature, it is ready.
[0057] In some embodiments, in step 1), the ratio of compound 1 to diethyl ketomalonate is 1:1-3 to synthesize the target probe BTNPO.
[0058] In some embodiments, in step 2), the reaction temperature is 30-118° C., and the reaction time is 8-18 hours, so as to improve the reaction efficiency.
[0059] In some embodiments, in step 2), the reaction temperature is 90-118° C., and the reaction time is 12-15 hours, so that higher reaction rate and yield can be obtained.
[0060] In some embodiments, step 2) also includes the steps of spinning the reaction product solution to dryness and purifying, so as...
Embodiment 1
[0071] Embodiment 1: the synthesis of fluorescent probe
[0072] Compound 1 (274 mg, 1 mmol) was dissolved in 3 mL of glacial acetic acid, and the above mixture was heated to reflux. Then, a solution of diethyl ketomalonate (348 mg, 2 mmol) in glacial acetic acid (2 mL) was added dropwise to the above mixed solution, and reacted for 15 h. After the reaction was completed, the reaction solution was cooled to room temperature, concentrated and spin-dried to dry the solvent, and the solid was subjected to column chromatography (eluents were dichloromethane:methanol:triethylamine=100:1:1, V / V / V) The product solids were obtained in 324 mg (yield 65%), respectively.
[0073] Mass Spectrometry and NMR Characterization:
[0074] BTNPO: HRMS (ESI): calculated for C 22 h 15 N 2 o 4 S - (M-H) - 403.0747, found 403.0747.
[0075] 1 H NMR (400MHz, DMSO-d 6 )δ10.92(s,1H),8.69(s,1H),8.22(t,J=8.3Hz,2H),8.17(d,J=8.0Hz,1H),8.09(d,J=8.1Hz, 1H), 7.96(d, J=8.8Hz, 1H), 7.57(t, J=7.6Hz, ...
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