Preparation method of Meso-tetra(3,4-dihydroxy phenyl) zinc porphyrin

A technology of dihydroxyphenyl and porphyrin zinc is applied in the preparation field of Meso-tetraporphyrin zinc, and achieves the effects of increasing diversity, simple preparation method and high yield

Inactive Publication Date: 2016-09-21
GUANGDONG UNIV OF TECH
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  • Application Information

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Problems solved by technology

[0002] First of all, the synthesis of Meso-tetrakis(3,4-dihydroxyphenyl)...

Method used

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  • Preparation method of Meso-tetra(3,4-dihydroxy phenyl) zinc porphyrin
  • Preparation method of Meso-tetra(3,4-dihydroxy phenyl) zinc porphyrin
  • Preparation method of Meso-tetra(3,4-dihydroxy phenyl) zinc porphyrin

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Embodiment 1

[0025] The invention provides a method for preparing Meso-tetrakis (3,4-dihydroxyphenyl) porphyrin zinc, comprising the following steps:

[0026] (1) Synthesis of Meso-tetrakis (3,4-dihydroxyphenyl) porphyrin (OOHPP) (such as figure 1 shown):

[0027] In a 250mL three-necked flask equipped with a condenser, a thermometer and a constant pressure dropping funnel, add 45mL of nitrobenzene, add zeolite, and heat to reflux; then weigh 1.5g of 3,4-dihydroxybenzaldehyde and dissolve it in 10mL Slowly drop the mixed solution of nitrobenzene and 7.5mol isobutyric acid into a three-necked flask, and reflux at a temperature of 135°C; after 20 minutes, slowly add freshly distilled pyrrole (1.3mL) and nitrobenzene (25mL) dropwise and the mixed solution was added dropwise within 30 minutes; the reaction solution quickly changed from light yellow to purple black, refluxed for 2 hours, and stopped heating; when the mixed solution was cooled to below 80°C, it was left to stand for 8 hours; A...

Embodiment 2

[0030] The characterization of embodiment 2 Meso-tetrakis (3,4-dihydroxyphenyl) porphyrin zinc

[0031] The characterization methods mainly include infrared spectroscopy, ultraviolet-visible spectroscopy, fluorescence spectroscopy and electron paramagnetic resonance spectroscopy. Among them, when measuring the ultraviolet-visible absorption spectrum, the solvent is CH 2 Cl 2 or CH 3 OH, the measurement range is 350-700nm; the infrared spectrum is detected by the Avatar370 FT-IR infrared spectrometer, and the potassium bromide (KBr) tablet is used, and the measurement range is 4000-400cm -1 ; The fluorescence spectrum is detected by a Fluorescence-max4 type fluorescence spectrometer, and the selected solvent has CH 2 Cl 2 、CH 3 OH and DMF, the grating interval is set to 3nm; the electron paramagnetic resonance spectrum is obtained by detecting the porphyrin solid with a type A200-9.5 / 12 electron paramagnetic resonance spectrometer.

[0032] Analysis of Meso-Tetrakis(3,4-D...

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Abstract

The invention discloses a preparation method of Meso-tetra(3,4-dihydroxy phenyl) zinc porphyrin and belongs to the technical field of chemical synthesis and detection. The preparation method of Meso-tetra(3,4-dihydroxy phenyl) zinc porphyrin adopts raw materials in proportion as follows: 1.5 g of 3,4-dihydroxy benzaldehyde, 1.3 mL of pyrrole, 80 mL of nitrobenzene, 7.5 mL of isobutyric acid, 0.40 g of zinc acetate, 35 mL of tetrahydrofuran and 5-10 mL of methanol. The preparation method is simple, and the yield of Meso-tetra(3,4-dihydroxy phenyl) zinc porphyrin is high.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and detection, in particular to a preparation method of Meso-tetrakis(3,4-dihydroxyphenyl)porphyrin zinc. Background technique [0002] First of all, the synthesis of Meso-tetrakis(3,4-dihydroxyphenyl)porphyrin zinc has never appeared in the literature, and it is a new substance. [0003] Secondly, the present invention provides an effective method for synthesizing Meso-tetrakis(3,4-dihydroxyphenyl)porphyrin zinc, and it is verified by a series of characterization means. Contents of the invention [0004] The object of the present invention is to overcome the shortcomings and deficiencies in the above-mentioned prior art, and provide a method for preparing Meso-tetrakis(3,4-dihydroxyphenyl)porphyrin zinc. [0005] The object of the present invention is achieved through the following technical scheme: a kind of preparation method of Meso-tetrakis (3,4-dihydroxyphenyl) porphyrin zinc, ...

Claims

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Application Information

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IPC IPC(8): C07D487/22C09K11/06
CPCC07D487/22C09K11/06C09K2211/188
Inventor 陈小婷吴雅红佟珊玲阎雁叶飞袁健林慧
Owner GUANGDONG UNIV OF TECH
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