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Azasilyl tricyclic salicylaldehyde zinc complex and its synthesis method

A technology of silicon nitrogen tricyclic and zinc complexes, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, chemicals for biological control, etc. Quasi-complexes, stuck in theoretical research and other issues

Active Publication Date: 2021-07-20
HUAIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, at present, the nitrogen silicon tricyclic complexes are still in the theoretical research stage, and there is no method for preparing the nitrogen silicon tricyclic complexes.

Method used

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  • Azasilyl tricyclic salicylaldehyde zinc complex and its synthesis method
  • Azasilyl tricyclic salicylaldehyde zinc complex and its synthesis method
  • Azasilyl tricyclic salicylaldehyde zinc complex and its synthesis method

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preparation example Construction

[0032] The invention provides a method for synthesizing a nitrogen-silicon tricyclic salicylaldehyde zinc complex. The synthetic method of this nitrogen silicon tricyclic salicylaldehyde zinc complex comprises the following steps:

[0033] (1) Take triethanolamine to react with γ-aminopropyltriethoxysilane. The reaction of triethanolamine and γ-aminopropyltriethoxysilane includes the following steps: add triethanolamine and γ-aminopropyltriethoxysilane into the first reaction vessel such as a round bottom flask, and keep the temperature at 120°C-140°C Under stirring, reaction 3h-4h.

[0034] The reaction product of triethanolamine and γ-aminopropyltriethoxysilane is subjected to atmospheric distillation to remove ethanol in the reaction product, and the residue after atmospheric distillation is subjected to vacuum distillation, and the oil bath for vacuum distillation The temperature was 220°C, and the first intermediate product was obtained.

[0035] Atmospheric distillati...

Embodiment 1

[0052] This example provides a method for synthesizing a nitrogen-silicon tricyclic salicylaldehyde zinc complex, which includes the following steps:

[0053] (1) Take triethanolamine to react with γ-aminopropyltriethoxysilane. The reaction of triethanolamine and γ-aminopropyltriethoxysilane includes the following steps: adding triethanolamine and γ-aminopropyltriethoxysilane into a first reaction vessel, stirring at a constant temperature of 130° C., and reacting for 3 hours.

[0054] A reflux device with a drying tube is installed on the first reaction vessel, and the drying tube is filled with calcium chloride, and the reaction product of triethanolamine and γ-aminopropyltriethoxysilane undergoes atmospheric distillation, and the temperature of the atmospheric distillation is Ethanol in the reaction product is distilled at 90°C, and the residue after atmospheric distillation is subjected to vacuum distillation. The oil bath temperature of vacuum distillation is 220°C, and t...

Embodiment 2

[0073] This example provides a method for synthesizing a nitrogen-silicon tricyclic salicylaldehyde zinc complex, which includes the following steps:

[0074] (1) Take triethanolamine to react with γ-aminopropyltriethoxysilane. The reaction of triethanolamine and γ-aminopropyltriethoxysilane includes the following steps: adding triethanolamine and γ-aminopropyltriethoxysilane into a first reaction vessel, stirring at a constant temperature of 130° C., and reacting for 3 hours.

[0075] A reflux device with a drying tube is installed on the first reaction vessel, and the drying tube is filled with calcium chloride, and the reaction product of triethanolamine and γ-aminopropyltriethoxysilane undergoes atmospheric distillation, and the temperature of the atmospheric distillation is Ethanol in the reaction product is distilled at 90°C, and the residue after atmospheric distillation is subjected to vacuum distillation. The oil bath temperature of vacuum distillation is 220°C, and t...

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Abstract

The invention discloses a nitrogen-silicon tricyclic salicylaldehyde zinc complex and a synthesis method thereof. The synthesis method comprises the following steps: taking triethanolamine to react with γ-aminopropyltriethoxysilane, and the reaction product is subjected to atmospheric distillation and vacuum distillation to obtain the first intermediate product; the first intermediate product is dissolved in anhydrous tetrahydrofuran to obtain the second intermediate product A solution, dropwise adding salicylaldehyde or 3-substituted salicylaldehyde or 4-substituted salicylaldehyde into the first solution, react at room temperature, and precipitate crystals after cooling, and process the precipitated crystals through a mixed solution of benzene and ether recrystallization to obtain recrystallization, and purification to obtain the second intermediate product; take zinc acetate and dissolve it with anhydrous methanol to obtain the second solution, get the second intermediate product and dissolve it with anhydrous tetrahydrofuran to obtain the third solution, and mix the second solution with The third solution is mixed and then reacted to precipitate solid matter, which is purified to obtain the zinc complex of azasilazine tricyclic salicylaldehyde. The synthesis method has low cost, few by-products and little environmental pollution.

Description

technical field [0001] The invention relates to a nitrogen silicon tricyclic salicylaldehyde zinc complex and a synthesis method thereof. Background technique [0002] Azasilatricyclic compounds have immune enhancement and anti-tumor effects, and have obvious effects on promoting cell proliferation and wound healing. Asazo-silicon tricyclic compounds such as some Schiff bases not only have good bactericidal and anticancer effects, but also have analgesic, anti-inflammatory, antibacterial and sterilizing, antiviral and other activities. The N atom of N has a lone pair of electrons, so various functional groups can be introduced into the Schiff base structure to derivatize it, which is unique in application. Salicylaldehyde has analgesic, anti-inflammatory, antibacterial, sterilizing, and antiviral activities, and is an effective herbicide, insecticide, and fungicide. At present, in the field of complexes, the synthesis of azanitrosilicon tricyclic compounds and salicylaldeh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18A61P31/04A01P1/00
CPCA61P31/04C07F7/1892
Inventor 胡扬剑欧阳跃军吕家远
Owner HUAIHUA UNIV