Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A method for microwave solid-phase synthesis of tetrabenzoporphyrin zinc (ii)

A technology for tetrabenzoporphyrin and solid-phase synthesis, which is applied in directions such as organic chemistry, and can solve the problems of low yield, complicated operation, and many operation steps.

Active Publication Date: 2021-07-06
HUANGGANG NORMAL UNIV
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These conventional synthetic methods have many operating steps, long reaction times and low yields.
Due to the serious sublimation of the solid direct heating method, the yield is not high (up to 15%), and there are also disadvantages such as complicated operation, long reaction time, and difficult separation and purification.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A method for microwave solid-phase synthesis of tetrabenzoporphyrin zinc (ii)
  • A method for microwave solid-phase synthesis of tetrabenzoporphyrin zinc (ii)
  • A method for microwave solid-phase synthesis of tetrabenzoporphyrin zinc (ii)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Microwave Synthesis of Zinc(Ⅱ) Tetrabenzoporphyrin

[0026] Weigh 0.19g (18mmol) malonic acid, 0.33g (18mmol) potassium phthalimide and 0.75g (3.75mmol) zinc acetate in a mortar, mix and grind for 5min, transfer the mixed powder to a 150mL round bottom flask , the microwave power is 800W radiation, the reaction is completed for 5min, the reaction is completed, and the reaction is taken out, and the crude product is obtained by cooling in the dark. The crude product is separated by column chromatography to obtain the refined product. Yield was 30%.

[0027] This method is used for synthesis, because the reaction speed is fast, the reaction time is short, and there is no sublimation phenomenon. The conventional method is to fully grind the raw materials and mix them evenly, first place the powder on a quartz boat, then put it into a quartz tube, and react at 400 °C for 60 min under argon protection, with a yield of 15%. It can be seen from the comparison that this meth...

Embodiment 2

[0029] Product map verification

[0030] Infrared spectrum verification: figure 1 The infrared spectrum of the tetrabenzoporphyrin zinc (II) prepared in Example 1 is shown. From the analysis of the figure, it can be seen that 1400cm -1 ~1600cm -1 The strong absorption peaks can be attributed to the characteristic absorption peaks of C=C and C=N in the porphyrin molecule, 1340cm -1 is the stretching vibration absorption peak of C-N.

[0031] UV spectrum verification: figure 2 The ultraviolet spectrum of the tetrabenzoporphyrin zinc (II) prepared in Example 1 is shown. From the analysis of the figure, it can be seen that it has strong absorption at 424nm and 623nm, and the strong absorption peak at 424nm is Porphyrin Soret band characteristic peak, the absorption peak at 623nm is the Q band absorption peak.

[0032] NMR verification: 1 H NMR: 7.89(m,2H), 7.78(m,4H), 7.71(d,2H), 7.57(m,4H), 7.35(m,3H), 7.19(m,4H), 7.02(d,1H) ).

[0033] It can be known from the above spe...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for synthesizing tetrabenzoporphyrin zinc(II) in solid phase by microwave, which comprises the following preparation steps: (1) weighing malonic acid, potassium phthalimide and zinc acetate, mixing and grinding The mixed powder is obtained; (2) the mixed powder is irradiated with microwaves until the reaction is complete to obtain a reactant; (3) the reactant is cooled in the dark and then separated by column chromatography. Beneficial effects of the present invention: (1) the reaction is carried out in a solid phase, the reaction environment is relaxed, the reaction conditions are limited, and the applicability is strong; (2) the microwave three-dimensional heating reaction is used to effectively shorten the reaction time and reduce the reaction energy barrier, without The thermal sublimation phenomenon improves the yield; (3) the reaction does not require a solvent, which can avoid the use and recovery of the solvent, and reduces the cost; (4) no solvent participates in the reaction, which is beneficial to purification.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for synthesizing zinc (II) tetrabenzoporphyrin. Background technique [0002] Metal porphyrin compounds and their derivatives are a class of macrocyclic aromatic compounds with 18r electronic structure. They are widely used in cancer diagnosis and recognition, catalysis, photocells, molecular recognition, photosensitivity materials and other fields. It can also simulate physiological processes in living organisms and deal with NO in automobile exhaust x Wait. [0003] At present, the methods of synthesizing metal porphyrin compounds include Alder synthesis method, Lindesy synthesis method, Guo Cancheng's new synthesis method and new method improved by Gaode. These conventional synthetic methods have many operation steps, long reaction time and low yield. The solid direct heating method has the disadvantages of serious sublimation, low yield (up to 15%), co...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 杨水彬周庆张玉洁张雪梅
Owner HUANGGANG NORMAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com