Method for synthesizing mu-oxo binuclear ferriporphyrin

A technology of iron porphyrin and oxobi is applied in iron organic compounds, organic chemistry and other directions, which can solve the problems of serious environmental pollution, long metallization time, difficult separation and purification, etc., to reduce pollution, shorten reaction time, and facilitate purification. Effect

Inactive Publication Date: 2008-07-23
BEIJING UNIV OF TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Obviously, the operation procedure is not only cumbersome, but also consumes a lot of energy and solvent, and does not fundamentally solve the problem that μ-oxybinuclear iron porphyrin cannot be synthesized in an acidic system.
[0006] (2) highly toxic nitrobenzene or its derivatives are used in the reaction, causing serious environmental pollution
[0007] (3) The metallization time is longer, at least 30 minutes or more
[0008] (4) before the method carries out the third step (reaction formula [c]) reaction, all fatty acids must be steamed out, as a result, unreacted ferrous salt is separated out, and mixed in the solid product that part crystallizes out, difficult for separation and purification

Method used

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  • Method for synthesizing mu-oxo binuclear ferriporphyrin
  • Method for synthesizing mu-oxo binuclear ferriporphyrin
  • Method for synthesizing mu-oxo binuclear ferriporphyrin

Examples

Experimental program
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Effect test

Embodiment 1

[0028] In a 250mL three-necked flask, add a mixed solvent of 1mL acetic acid and 99mL DMF (both volume percentages are 1% and 99%, respectively), add 1mmol porphyrin ligand and 1mmol ferrous sulfate, heat and reflux for 5min, cool to room temperature and add 20mL water, suction filtration, wash filter cake with ethanol and water, dry, obtain μ-oxo binuclear iron porphyrin (being R in general formula (II) 1 = H, R 2 = H, R 3 =H), the yield was 95%.

Embodiment 2

[0030] In a 250mL three-necked flask, add a mixed solvent of 20mL acetic acid, 10mL caprylic acid and 70mL DMF (the three volume percentages are 20%, 10%, 70%, respectively), add 1mmol p-methylporphyrin ligand and 1.5mmol ferrous acetate , heating to reflux for 0.5min, cooling to room temperature, adding 5mL of water, suction filtration, washing the filter cake with ethanol and water, and drying to obtain μ-oxo-p-methylbinuclear iron porphyrin (i.e. R in the general formula (II) 1 =CH 3 , R 2 = H, R 3 =H), the yield was 97%.

Embodiment 3

[0032] In a 250mL three-neck flask, add 50mL propionic acid, 50mL DMF (50% and 50% by volume respectively) mixed solvent, add 1mmol o-chloroporphyrin ligand and 3mmol ferrous acetate, heat to reflux for 1min, and cool to room temperature Then add 50mL water, suction filter, wash the filter cake with ethanol and water, and dry to obtain μ-oxo-o-chlorobinuclear iron porphyrin (i.e. R in the general formula (II) 1 = H, R 2 = H, R 3 =Cl), the yield was 93%.

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Abstract

The invention relates to a synthetic method for Mu-oxo dinuclear iron porphyrin, which comprises the steps that the porphyrin ligand and the soluble ferrous salt are adopted as the material; the mixed liquid of at least one of C2 to C8 straight chain fatty acids with the volume percentage of 1% to 80% and DMF is adopted as the solvent; the solution with the dissolved porphyrin ligand and soluble ferrous salt is heated and refluxed for 0.5 to 5 min, then is cooled to the ambient temperature; the water of 5 to 50 ml is added; finally the Mu-oxo dinuclear iron porphyrin is obtained after separation and purification. The synthetic method for Mu-oxo dinuclear iron porphyrin has the advantages of direct adoption of acid medium, simple operation, environmental friendliness, short reaction time and easy separation and purification of the product.

Description

technical field [0001] The invention relates to a synthesis method of μ-oxo binuclear iron porphyrin. Background technique [0002] μ-oxo-binuclear iron porphyrin can catalyze the selective oxidation of hydrocarbons to synthesize organic intermediates under mild conditions, and has been successfully applied in industrial production. Therefore, the research on the synthetic method of μ-oxobinuclear iron porphyrin is not only of great theoretical significance, but also has a broad prospect of industrial application. [0003] The existing research results show that μ-oxo-binuclear iron porphyrin can be easily converted into corresponding mononuclear iron porphyrin under acidic conditions. Therefore, researchers in the field generally believe that μ-oxo-binuclear iron porphyrin can only be synthesized under neutral or alkaline conditions, but cannot be synthesized under acidic conditions by porphyrin ligands and ferrous salts. [0004] Patent CN101050218 (disclosure date: Octo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22C07F15/02
Inventor 佘远斌王爱欣冯连顺樊静钟儒刚
Owner BEIJING UNIV OF TECH
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