Method for synthesizing mu-oxo binuclear ferriporphyrin
A technology of iron porphyrin and oxobis, which is applied in the fields of iron-organic compounds and organic chemistry, can solve problems such as difficult separation and purification, cumbersome operating procedures, and serious environmental pollution, and achieve shortened reaction time, simplified operating procedures, and reduced pollution Effect
Inactive Publication Date: 2010-08-18
BEIJING UNIV OF TECH
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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.
(2) highly toxic nitrobenzene or its derivatives are used in the reaction, causing serious environmental pollution
(3) The metallization time is longer, at least 30 minutes or more
(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
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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 The invention relates to a synthesis method of μ-oxo binuclear iron porphyrin. Background technique 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. 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. Patent CN101050218 (disclosure date: October 10, 2007) discloses a synthe...
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Patent Type & Authority Patents(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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