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Novel solid-state phase transfer catalyst based on Cd-MOF, method for preparing novel solid-state phase transfer catalyst and application thereof

A cd-mof-1, C27H19N4O2 technology, applied in the field of catalyst preparation, can solve the problems of complicated operation, difficult catalyst recovery and high cost

Inactive Publication Date: 2016-06-29
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, phase transfer catalysts have been widely used in most fields of organic reactions, such as carbene reaction, substitution reaction, oxidation reaction, reduction reaction, diazotization reaction, displacement reaction, alkylation reaction, acylation reaction, polymerization reaction, and even Polymer modification, etc.; however, the above method has problems such as difficult catalyst recovery, high cost, and complicated operation

Method used

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  • Novel solid-state phase transfer catalyst based on Cd-MOF, method for preparing novel solid-state phase transfer catalyst and application thereof
  • Novel solid-state phase transfer catalyst based on Cd-MOF, method for preparing novel solid-state phase transfer catalyst and application thereof
  • Novel solid-state phase transfer catalyst based on Cd-MOF, method for preparing novel solid-state phase transfer catalyst and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Embodiment 1: the preparation of organic ligand L

[0075] Concrete preparation steps are as follows:

[0076] (1) 4,4-dibromobenzil (10.00g, 27.17mmol), ammonium acetate (41.89g, 543.45mmol), paraformaldehyde (1.63g, 54.34mmol), join in 100mL glacial acetic acid solution, stir Heat to reflux for 5 hours, adjust to neutral with saturated sodium carbonate solution after the reaction, extract with 200mL ethyl acetate, wash with sodium carbonate solution, extract the aqueous phase with ethyl acetate, combine the organic phases, and wash with anhydrous magnesium sulfate Dry, filter, and remove the solvent under reduced pressure to obtain 10.07 g of a yellow solid with a yield of 98.00%.

[0077]

[0078] (2)N 2 Under protection, intermediate A (10.58mmol, 4.00g) and sodium hydride (11.64mmol, 0.28g) were placed in a 100ml three-necked flask, and 50ml of anhydrous THF was slowly added as a solvent, heated to 80°C, and stirred at a constant temperature of 80°C for 1h , ...

Embodiment 2

[0083] Embodiment 2: the synthesis of Cd-MOF-1

[0084] The organic ligand L (8.60mg, 0.02mmol) prepared in Example 1 and cadmium acetate (0.01mmol, 2.13mg) were dissolved in 2mL of methanol, placed in a 5ml small test tube, and kept at 120°C for 72 hours. After 50 hours, the temperature was cooled to room temperature to obtain colorless blocky crystals [Cd(C 27 h 19 N 4 o 2 ) 2 ] n , n is a non-zero natural number, the yield is 4.3 mg, and the yield is 44% (based on L).

[0085] We characterized the compound by IR and TGA, and the results are shown in 10 and 11, respectively.

Embodiment 3

[0086] Example 3: Synthesis of Cd-MOF-1'

[0087] Put the Cd-MOF-1,1-bromopropane prepared in Example 2 into a 25ml two-necked bottle, add 10ml of anhydrous acetonitrile as a solvent, heat to 80°C-90°C, stir for 48 hours, stop heating, and let the reaction system decompose. to room temperature, centrifuged, collected the precipitate, washed twice with acetonitrile, washed twice with methanol, and washed twice with ether to obtain a three-phase catalyst metal-organic framework Cd-MOF-1′, which we characterized by IR and TGA , see the results respectively Figure 12 , 13 .

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Abstract

The invention discloses a novel solid-state three-phase catalyst. The novel solid-state three-phase catalyst comprises organic ligands L for synthesizing metal organic frameworks based on Cd(II), metal organic frameworks Cd-MOF-1 based on Co(II) and metal organic frameworks Cd-MOF-1' based on Co(II). A method for preparing the novel solid-state three-phase catalyst includes synthesizing the metal organic frameworks Cd-MOF-1 by the aid of the organic ligands L; arranging the metal organic frameworks CD-MOF-1 and 1-dodecyl bromide in a double-opening flask with the volume of 25 ml, adding 10 ml of anhydrous acetonitrile into the double-opening flask and heating the metal organic frameworks CD-MOF-1, the 1-dodecyl bromide and the anhydrous acetonitrile until the temperatures of the metal organic frameworks CD-MOF-1, the 1-dodecyl bromide and the anhydrous acetonitrile reach 80-90 DEG C; carrying out stirring reaction on the metal organic frameworks CD-MOF-1, the 1-dodecyl bromide and the anhydrous acetonitrile for 48 h; stopping heating the metal organic frameworks CD-MOF-1, the 1-dodecyl bromide and the anhydrous acetonitrile; arranging reaction systems in room-temperature environments; centrifugally separating the reaction systems; collecting precipitates; washing the precipitates by the aid of acetonitrile twice; washing the precipitates by the aid of methanol twice; washing the precipitates by the aid of diethyl ether twice to obtain the novel solid-state three-phase catalyst Cd-MOF-1'. The anhydrous acetonitrile is used as a solvent. The novel solid-state three-phase catalyst has the advantages that azidation reaction on 1-bromobutane can be effectively catalyzed by the novel solid-state three-phase catalyst without reaction of the traditional phase transfer catalysts, the reaction temperature is mild, and the novel solid-state three-phase catalyst is short in reaction time, low in usage and free of other additives, is easy to recycle as compared with the traditional phase transfer catalysts and can be reused by more than three times.

Description

technical field [0001] The invention relates to a metal-organic framework based on Cd(II) and its preparation, post-modification method and application, and belongs to the technical field of catalyst preparation. Background technique [0002] Metal-organic Framework (MOF) is a research hotspot in recent years. Compared with traditional porous materials, MOFs are a new type of porous organic-inorganic hybrid solid materials with a wide range of applications. MOFs have special topology. Pores with a structure, internal regular arrangement, and fixed size and shape. The design, synthesis and performance expression of coordination-driven supramolecular systems have become the main theme of research on organic-inorganic coordination compounds. With the progress of research, the design synthesis and post-modification and catalytic properties of MOFs have attracted more and more attention. [0003] Heterogeneous organic reactions are often encountered in organic synthesis, and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/08B01J31/22C07C247/04
CPCB01J31/2217B01J2231/4277B01J2531/0241B01J2531/27C07C247/04C07F3/003
Inventor 董育斌王建成马建平刘启奎胡玉红
Owner SHANDONG NORMAL UNIV
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