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Nano-cluster and its preparation method and application

A nanocluster, reaction technology, applied in chemical instruments and methods, fluorescence/phosphorescence, luminescent materials, etc., can solve problems such as lack of water-soluble probes

Active Publication Date: 2016-01-06
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, there is still a lack of water-soluble probes that can highly selectively recognize iron ions with specific oxidation states and can be applied in practical biological systems.

Method used

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  • Nano-cluster and its preparation method and application
  • Nano-cluster and its preparation method and application
  • Nano-cluster and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1, the preparation of coordination compound MD

[0038] Weigh 0.28mmol of IrCl 3 ·H 2 O and 2.0 mmol of NaAc were dissolved in 200 mL of 1,2-propanediol, heated to reflux at 165° C. for reduction reaction for 1 h, and after cooling to room temperature, 200 μL of toluene solution of dodecyne was added (the molar weight of dodecyne was 0.84 mmol), After stirring for ligand exchange reaction for 24 hours, liquid separation and suction filtration were dried to obtain a black powder. The transmission electron microscope image shows that the particle size of the nanoparticle MD is 1.2±0.4nm.

[0039] 1 HNMR (300MHz, CDCl 3 ): δppm0.9 (s, CH 3 ), 1.2 (s, CH 2 ).

[0040] It can be seen from the above that the single peak at 0.9ppm is attributed to the dodecyne terminal methyl-CH 3 The proton splitting peak of the dodecyne monomer, although the methyl proton at the end of the dodecyne monomer is triple splitting, but after being modified on the iridium nanopa...

Embodiment 2

[0041] The preparation of 2-(2-pyridylmethyl)-4-vinylphenethylamine shown in embodiment 2, formula I

[0042] Weigh 1.3g (8.0mmol) 4-chloromethylstyrene, 1.0g (5.0mmol) 2-(2-pyridylmethyl) amine and 4mL (40.0mmol) triethylamine and dissolve in 30mL of dichloromethane, Stir at room temperature for nucleophilic reaction for 8 hours, then filter with suction and distill under reduced pressure to obtain a light yellow liquid with a yield of 68%.

[0043] 1 HNMR (300MHz, CDCl 3 ): δppm3.59 (s, 2H, NCH 2 Ph), 3.73(s, 4H, pyCH 2 ), 5.12 (d, 1H, cis-CH 2 CH), 5.60 (1H, trans-CH 2 CH), 6.60 (dd, 1H, CH 2 CH), 7.0-7.6(m, 10H, aromaticH), 8.41(m, 2H, pyH 6 ).

[0044] Infrared spectrum (KBr tablet, cm -1 ): v=2974, 2938(aromaticC-H), 1629(C=C), 1589, 1568(aromaticC=C), 1261, 1096(C-N), 803(=C-H),

[0045] Mass spectrum: m / z (%) 316.2 (C 21 h 21 N 3 ).

[0046] From the above, it can be seen that the product has a correct structure and is the target compound.

Embodiment 3

[0047] Embodiment 3, the preparation of iridium nanocluster ML (the feeding mass ratio x of the compound shown in MD and formula I: y is 1: 1)

[0048] Weigh 30 mg of the obtained compound MD prepared in Example 1 and 30 mg (0.10 mmol) of the ligand compound shown in Formula I prepared in Example 2 and dissolve it in 50 mL of anhydrous dichloromethane, stir at room temperature for olefin metathesis reaction for 2 days, and filter with suction. The obtained solid was washed several times with ethanol to obtain iridium nanoparticles, and then its photophysical properties were measured.

[0049] The transmission electron microscope image shows that the average particle size of the iridium nanocluster is 1.3±0.4nm.

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Abstract

The invention discloses a nanocluster, as well as a preparation method and application thereof. The preparation method of the nanocluster provided by the invention comprises the following steps of: evenly mixing a coordination compound with a compound shown in ligand in a formula I to carry out olefin crossmetathesis, so as to obtain the nanocluster after the reaction is finished, wherein the light-emitting wavelength of the nanocluster can be adjusted along with different ratios of surface functional group. The invention further provides an application of the nanocluster in detection of a ferric ion. The nanocluster provided by the invention can be used for achieving high-selectivity and high-sensitivity detection of the ferric ion, thus providing possibility for building a fluorescent chemical sensor for high-selectivity and high-sensitivity detection of the ferric ion. The iridium nanocluster provided by the invention can be used for not only imaging cell endogenous Fe<3+>, but also detecting exogenous Fe<3+>, and is expected to be used for detection of Fe<3+> in physiological and pathological processes.

Description

technical field [0001] The invention relates to a nano-cluster, a preparation method and application thereof. Background technique [0002] Iron is an essential trace element for the human body. It maintains a dynamic balance in the body in various forms and is a metal element necessary for the normal growth of almost all biological cells. Iron in the human body mainly exists in the form of hemoglobin in circulating red blood cells and participates in the synthesis of hemoglobin, cytochrome and various enzymes, and plays a vital role in maintaining the balance of metabolism in the human body. Too low or too high iron ion content will cause a series of diseases. When iron ion is deficient, it will lead to many metabolic disorders such as oxygen transportation and storage, carbon dioxide transportation and release, electron transfer, redox, and damage the immune mechanism of the body. , resulting in many physiological and pathological changes; when iron ions are excessive, it...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00C07D213/36C09K11/06G01N21/64
Inventor 毛兰群杨丽芬姜琴
Owner INST OF CHEM CHINESE ACAD OF SCI
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