A kind of fluorescent probe with AIE effect and its preparation method and application
A fluorescent probe and effect technology, applied in the field of fluorescent probes, can solve problems such as poor selectivity, poor photobleaching resistance, and high biological toxicity, and achieve the effect of improving the possibility
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0050] With a double-necked flask, 2.0004g (8.1mmol) of 1-pyrene boronic acid, 3.0000g (8.95mmol) of triphenylbromoethylene and 0.5000g K 2 CO 3 dissolved in 40 mL of ethylene glycol dimethyl ether and 20 mL of H 2 O after N 2 Under protection, 0.1400 g (0.12 mmol) of tetrakistriphenylphosphine palladium was added, and heated to reflux at 40-60° C. for 15-20 h. Ethylene glycol dimethyl ether was removed by a rotary evaporator and filtered under reduced pressure to obtain a green crude product. Chromatography with n-hexane: ethyl acetate = 8:1 as the eluent gave 1-(1,2,2-triphenylethenyl)pyrene as a blue-green powdery solid with a yield of 36.21%.
[0051] 1-(1,2,2-triphenylethenyl)pyrene's proton nuclear magnetic resonance spectrum measurement results are: 1H NMR (400MHz, DMSO-d6) δ = 8.35 (d, 1H, J = 8Hz), 8.27 (d ,1H,J=8Hz), 8.22(d,1H,J=8Hz), 8.15(m,5H), 7.89(d,1H,J=8Hz), 7.27(m,5H), 7.06(m,5H) , 6.98 (d, 2H, J=8Hz), 6.88 (m, 3H).
Embodiment 2
[0053]Dissolve 0.2740g (0.6mmol) of 1-(1,2,2-triphenylethenyl)pyrene in 5mL of dichloromethane, heat and stir until clear, and slowly add 100μL65 diluted with 0.2mL acetic acid dropwise under ice bath %-68% mixed solution of nitric acid. After 1 to 2 hours, heat and reflux for 4 to 5 hours. After the reaction reaches the limit as detected by TLC, use saturated NaHCO 3 Extract, filter under reduced pressure, and spin dry the solvent. The compound of formula (Ⅲ) was obtained as a yellow solid by column chromatography with the eluent of n-hexane:dichloromethane=2:1, specifically 1-nitro-8-(1,2,2-triphenyl A mixture of vinyl)pyrene and 1-nitro-6-(1,2,2-triphenylethenyl)pyrene with a yield of 85.01%.
Embodiment 3
[0055] 0.5000g (1mmol) of 1-nitro-8-(1,2,2-triphenylvinyl)pyrene and 1-nitro-6-(1,2,2-triphenyl) prepared in Example 2 The mixture of vinyl vinyl)pyrene was dissolved in 10mL of toluene:ethanol=1:1 mixed solvent, under N 2 Add 0.0800g (0.75mmol) of 10% Pd / C under protection, and slowly add 0.0600g (1.2mmol) of hydrazine hydrate dropwise after heating to reflux. After reacting for 4 to 5 hours, no raw materials were detected by TLC, and then filtered under reduced pressure, and the solvent was removed by rotary evaporation, and the compound of formula (II) was obtained as a yellow solid by column chromatography with the polarity of n-hexane: ethyl acetate = 3:1 8-(1,2,2-triphenylethenyl)pyrene-1-amine, the yield rate is 23.69%; Vinyl)pyrene-1-amine, the yield was 30.18%.
[0056] 8-(1,2,2-triphenylethenyl)pyrene-1-amine H NMR spectrum measurement results are: 1 HNMR (400MHz, DMSO-d6) δ = 8.16 (d, 1H, J = 12Hz), 8.02 (d, 1H, J = 8Hz), 7.94 (d, 1H, J = 8Hz), 7.84 (d, 2H, J = ...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


