Squaraine dye as well as preparation method and application thereof
A squaraine and dye technology, applied in organic dyes, chemical instruments and methods, methine-based/polymethine-based dyes, etc., can solve the problems of poor biological safety performance and slow metabolism of heavy metals, and achieve good fluorescence quantum yield, The effect of obvious reaction site and simple preparation method
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Embodiment 1
[0039] Embodiment 1, the synthesis of intermediate C
[0040]
[0041](1) Compound A (2.56g) was put into a round bottom flask containing 50ml DMF. After it was completely dissolved, sodium hydride (1.09g) was added in an ice-water bath. After stirring at room temperature for 5 minutes, n-butyl iodide was added. Alkane (4.27g), after stirring at room temperature for 2h, the reactant was washed with sodium chloride saturated water (2×50mL), then extracted with ethyl acetate and water (1:1 by volume), and the ethyl acetate layer After the solvent was removed by rotary evaporation, the crude product was obtained; the crude product was dissolved in 1 mL of ethyl acetate and used as a sample solution for silica gel column chromatography. Fill the chromatographic column (3cm×30cm) with 50g of 100-200mesh column chromatography silica gel and 50mL of ethyl acetate, release the ethyl acetate, slowly load the sample along the tube wall, and elute with ethyl acetate as the eluent. Th...
Embodiment 2
[0046] Embodiment 2, the synthesis of squaraine dye SQ890.
[0047]
[0048] Put the intermediate C (27mg) and squaraine (7mg) prepared by the method in Example 1 into a round-bottomed flask containing n-butanol (4ml) and toluene (4ml), heat and reflux at 110°C for 1h, and the reaction solution was rotary evaporated After removing the solvent, the concentrate was dissolved in 1 mL of dichloromethane and used as a sample solution for silica gel column chromatography. Fill a chromatographic column (3cm×30cm) with 50g of 100-200 mesh column chromatography silica gel and 50mL of dichloromethane, release the dichloromethane and slowly load the sample along the tube wall, and use dichloromethane as the eluent for elution. The off-rate is 1mL / min, the elution volume is 7 column volumes, the mixed solvent of dichloromethane and methanol (volume ratio is 10:1) is used as developing solvent for TLC monitoring, and the collected Rf value is 0.2-0.4 After the components of dichloromet...
Embodiment 3
[0052] Embodiment 3, squaraine dye absorption spectrum and emission spectrum detection
[0053] Ultraviolet-visible absorption spectrum test: adopt ultraviolet-visible light spectrophotometer (UV-5500PC, Shanghai Yuan Analysis Instrument Co., Ltd.) to carry out ultraviolet-visible absorption spectrum detection to the squarylium dye SQ890 prepared by the method of embodiment 2: take 300 μ L concentration to be 0.15mg / Place the SQ890 DMF solution of 1 ml in a quartz cuvette, set the DMF to zero as the baseline, and select the wavelength range of 650nm to 1100nm for spectral scanning. The results are shown in image 3 As shown, SQ890 has strong absorption between 750nm and 950nm.
[0054] Fluorescence emission spectrum test: adopt fluorescence spectrophotometer (PerkinElmer Lambda 750) to carry out fluorescence emission spectrum detection to squarylium dye SQ890 prepared by the method of embodiment 2: get 3ml concentration and be the SQ890DMF solution of 10 μ M, select 800nm~155...
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