Fluorescent material for five-membered heterocyclic compound specific detection and preparation method
A technology of fluorescent materials and five-membered heterocycles, applied in luminescent materials, magnesium organic compounds, nickel organic compounds, etc., can solve the problems of high cost, complicated pretreatment, time-consuming and labor-intensive, etc., and achieve rapid response and fast fluorescence response. , the effect of high yield
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Embodiment 1
[0038] (1) Preparation of TABD-COOH
[0039] 0.87g (4.75mmol) PdCl 2 and 3.28g (14.25mmol) CuBr 2 , into a 500mL round-bottomed flask, inject 5mL of acetonitrile and 250mL of toluene into the flask with a syringe, add 10.10g (99.02mmol) phenylacetylene at the same time, stir and react at room temperature for 24h, dry (the solvent acetonitrile and toluene are blown dry), and obtain Product 1; after dissolving product 1 with dichloromethane, wash with saturated ammonium chloride solution, separate liquids, dry the gained organic phase with anhydrous magnesium sulfate, suction filter, and spin dry to obtain product 2; Ether is the eluent, separated by column chromatography to obtain the product 3; the product 3 is recrystallized to obtain white needle-like crystals; wherein, dichloromethane is used as a good solvent for recrystallization, and petroleum ether is used as a poor solvent; recrystallization The specific process is: dissolve the product 3 with a very small amount of ...
Embodiment 2
[0061] (1) Preparation of TABD-COOH
[0062] TABD-COOH was prepared according to the method in step (1) of Example 1.
[0063] (2) TABD-MOF-2 (Mg 2 C 102 h 88 N 4 o 16 ) preparation
[0064] Add 0.045g TABD-COOH and 10mL N,N-dimethylformamide (DMF) into a 20mL beaker in turn, heat and stir until completely dissolved to obtain 0.01mol / L TABD-COOH DMF solution S1; add 0.026g Mg(NO 3 ) 2 ·6H 2 O and 5mL DMF were added to a 10mL beaker, and stirred at room temperature until completely dissolved to obtain 0.02mol / L Mg(NO 3 ) 2 ·6H 2 DMF solution S2 of O;
[0065] Add 1mL solution S1, 1mL solution S2, 0.5mL water and 0.5mL ethanol to a 5mL vial in turn, mix well, cap the vial tightly and put it in an oven at 85°C to react for 48h, filter, and wash 3 times with DMF to obtain a white tablet shape crystal, the crystal structure of white flake crystal obtained by X-ray single crystal diffraction is as follows Figure 5 ,From Figure 5 It can be seen that in this structure...
Embodiment 3
[0073] (1) Preparation of TABD-COOH
[0074] TABD-COOH was prepared according to the method in step (1) of Example 1.
[0075] (2)TABD-MOF-3(C 36 h 34 N 2 NiO 6 ) preparation
[0076] Add 0.045g TABD-COOH and 10mL N,N-dimethylformamide (DMF) into a 20mL beaker in turn, heat and stir until completely dissolved to obtain a DMF solution S1 of 0.01mol / L TABD-COOH; add 0.029g Ni(NO 3 ) 2 ·6H 2 O and 5mL DMF were added into a 10mL beaker, stirred at room temperature until completely dissolved to obtain 0.02mol / L Ni(NO 3 ) 2 ·6H 2 DMF solution S2 of O;
[0077] Add 1mL solution S1, 1mL solution S2, 0.5mL water and 0.5mL ethanol to a 5mL vial in sequence, mix well, cap the vial tightly and put it in an oven at 85°C to react for 28h, filter, and wash 3 times with DMF to obtain a white tablet shape crystal, the crystal structure of white flake crystal obtained by X-ray single crystal diffraction is as follows Figure 7 ,From Figure 7 It can be seen that in this structure,...
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