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5-isonicotinamidopyridylisotitanate cadmium complex, and preparation method and application thereof

A technology of isonicotinamide pyridyl iso-titanate cadmium and complexes is applied in the preparation of organic compounds, the preparation of carboxylic acid nitrile, cadmium organic compounds, etc., and achieves the effects of convenient operation, simple process and high yield

Active Publication Date: 2020-03-27
HENGYANG NORMAL UNIV
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Problems solved by technology

[0003] It has been reported in the literature that the simple fluorescence properties of 4-isonicotinamide pyridyl phthalate cadmium compounds have been reported. Some carboxylic acid compounds have the function of detecting cationic Fe(III). Catalyze the Knovevenagel condensation reaction, and the cadmium compound constructed from amide carboxylic acid can not only catalyze the Knovevenagel condensation reaction, but also have the function of fluorescent probe for large anions, which has not been reported so far

Method used

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  • 5-isonicotinamidopyridylisotitanate cadmium complex, and preparation method and application thereof
  • 5-isonicotinamidopyridylisotitanate cadmium complex, and preparation method and application thereof
  • 5-isonicotinamidopyridylisotitanate cadmium complex, and preparation method and application thereof

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preparation example Construction

[0025] The present invention also provides the preparation method of the cadmium 5-isonicotinamide pyridyl isotitanate complex, the steps are as follows: 5-isonicotinamide pyridyl isotitanate and cadmium salt are mixed in a molar ratio of 1-2:1- 2 Dissolve in an organic mixed solvent, heat up to 110-130°C to react, after the reaction is completed, cool and crystallize naturally, wash and dry the crystals to obtain the product.

[0026] In one embodiment, the cadmium salt is at least one of cadmium perchlorate and / or cadmium chloride.

[0027] In one embodiment, the organic mixed solvent is a mixed solvent of DMF and THF, and the volume ratio of DMF and THF is 1:1.

[0028] In one embodiment, the temperature increase rate during the temperature increase is 10° C. / h.

[0029] In one embodiment, the reaction time is 60-90 hours.

[0030] The present invention also provides the application of the cadmium 5-isonicotinamide pyridyl isotitanate complex in catalyzing the Knovevenage...

Embodiment 1

[0034] Dissolve 5-isonicotinamide pyridylisotitanic acid (28.7mg, 0.1mmol) and cadmium chloride (18.2mg, 0.1mmol) in DMF (5mL) and THF (5mL), seal them in a 16mL reaction vessel, and Heating at a rate of 10°C per hour to 120°C, maintaining this temperature for 3 days, and then cooling down to room temperature naturally, a colorless columnar crystal can be obtained, which is separated, washed and dried in sequence to obtain the target product, the yield About 40%.

[0035] The main infrared absorption peaks are: 3214m, 2926m, 2360m, 1618s, 1546s, 1429m, 1356m, 1278s, 1227s, 1089s, 1022m, 942s, 915s, 847s, 774s, 705m.

[0036] Catalytic performance experiment of the prepared cadmium complex:

[0037] Its catalytic reaction steps are as follows: add p-tolualdehyde (2.1mmol, 0.2425g) in the round bottom flask, malononitrile (2.0mmol, 0.1321g), catalyst 5-isonicotinamide pyridyl isotitanate cadmium complex ([Cd 2 (L) 2 (DMF)(THF)]·2DMF·THF)Cd-MOF (0.038g, 0.08mmol(3%)), wherein...

Embodiment 2

[0050] Dissolve 5-isonicotinamide pyridylisotitanic acid (43.1mg, 0.15mmol) and cadmium perchlorate (57.3mg, 0.15mmol) in DMF / THF (5mL each), seal them into a 16mL reaction kettle, and Heat to 110°C at a rate of 10°C per hour, maintain this temperature for 3 days, and then cool down to room temperature naturally to obtain colorless columnar crystals, which are separated, washed and dried in turn to obtain the target product with a yield of about 52%.

[0051] The 5-isonicotinamide pyridyl isotitanate cadmium complex catalyzes the heterogeneous reaction of p-tolualdehyde and malononitrile according to the steps and conditions of Example 1, and the conversion rate of p-tolualdehyde is 98.6%, and the catalyst After 3 cycles, the conversion rate of p-tolualdehyde does not decrease significantly, and the catalyst basically has no loss.

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Abstract

The invention discloses a 5-isonicotinamidopyridylisotitanate cadmium complex, and a preparation method and an application thereof, and belongs to the technical field of porous layered materials. Theporous complex has a two-dimensional double-layer network structure, the chemical expression of the porous complex is [Cd2(L)2DMFTHF].2DMF.THF, wherein L is a 5-isonicotinamidopyridylisotitanate ion.The preparation method comprises the following steps: carrying out a solvothermal reaction on 5-isonicotinamidopyridylisotitanic acid and a cadmium salt, and washing and drying the obtained reaction product to obtain the novel porous cadmium complex with a stable structure. The preparation method has the advantages of simple process, convenience in operation, and high yield; and the prepared 5-isonicotinamidopyridylisotitanate cadmium complex can selectively catalyze a Knoevenagel condensation reaction of p-tolualdehyde and malononitrile, has the characteristics of good selectivity and high catalytic activity as a catalyst, and can be used as a fluorescent probe for dichromate ions and permanganate ions.

Description

technical field [0001] The invention belongs to the technical field of porous layered materials, and in particular relates to a cadmium 5-isonicotinamide pyridyl isotitanate complex and a preparation method and application thereof. Background technique [0002] Metal-organic framework materials (MOFs) combine the characteristics of the structure design of organic ligands and the easy functionalization of inorganic complexes, increasing the selectivity of specific reactions and the purpose of fluorescence sensing. The ability of MOF to assemble well-defined molecular building blocks into a microporous framework is especially suitable for evenly distributing and immobilizing catalytically active organometallics in its open pores, making it highly efficient and easy to react. Double advantage of separation in the system. Generally, new MOFs can be constructed by using non-reporter and coordination sites or by using functionalized ligands. [0003] It has been reported in the ...

Claims

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Application Information

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IPC IPC(8): C07F3/08C07D213/81C09K11/06B01J31/22C07C253/30C07C255/34G01N21/64
CPCC07F3/003C07D213/81C09K11/06B01J31/2243C07C253/30G01N21/6428C09K2211/188C09K2211/1029C07B2200/13B01J2231/4205B01J2531/27C07C255/34
Inventor 陈满生张春华邓奕芳盛良兵孙俊彬卢伟红
Owner HENGYANG NORMAL UNIV
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