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Preparation method for ultraviolet absorbent

An absorber and ultraviolet technology, applied in the field of preparation of ultraviolet absorbers, can solve the problems of low yield, unsuitable for industrial production, low product purity, etc., and achieve the effects of high product yield, low cost and high product purity

Active Publication Date: 2019-10-18
安徽新秀化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] N-(2-ethoxyphenyl)-N'-(4-ethylphenyl)-oxalamide is a new type of ultraviolet absorber, which has a very good absorption effect on ultraviolet rays, and is also more and more popular Welcomed by the industry, the current conventional preparation method of N-(2-ethoxyphenyl)-N'-(4-ethylphenyl)-oxalamide has low yield and low product purity, which is not suitable for industrial production. Therefore for N-(2-ethoxyphenyl)-N'-(4-ethylphenyl)-oxalamide, it is very important to develop a preparation method that is easy to prepare, high in yield and suitable for industrial production.

Method used

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  • Preparation method for ultraviolet absorbent
  • Preparation method for ultraviolet absorbent
  • Preparation method for ultraviolet absorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method for an ultraviolet absorber, comprising the steps of:

[0037] (1) Synthesis of oxalamide ester intermediate:

[0038]

[0039] Add the dichloroethane solvent and the purchased ethyl oxalyl chloride raw material into the reaction bottle 1, heat up and stir, control the temperature in the reaction bottle 1 to 50°C, and add o-ethylaniline dropwise into the reaction bottle 1, wherein the oxalyl chloride ethyl The molar ratio of ester to o-ethylaniline is 2.5:1. After the reaction, cool down to normal temperature, add 5% sodium carbonate aqueous solution to wash until pH=8, then wash with water until neutral, and desolventize to obtain the oxalamide ester intermediate;

[0040] (3) Synthesis of N-(2-ethoxyphenyl)-N'-(4-ethylphenyl)-oxalamide product:

[0041]

[0042] Taking o-aminophenethyl ether and the oxalamide ester intermediate obtained in step (1) as raw materials, the molar ratio of the oxalamide ester intermediate and the anthranilamide ...

Embodiment 2

[0044] A preparation method for an ultraviolet absorber, comprising the steps of:

[0045] (1) the synthetic method of ethyl oxalyl chloride:

[0046]

[0047]Add oxalyl chloride in the reaction flask 1, control the temperature in the reaction flask to be -10°C, and add absolute ethanol dropwise to the reaction flask 1 under the condition of stirring, the molar ratio of the oxalyl chloride to the absolute alcohol is: 1:3, after the reaction, rectification and purification to obtain ethyl oxalyl chloride;

[0048] (2) Synthesis of oxalamide ester intermediate:

[0049]

[0050] Add the dichloroethane solvent and ethyl oxalyl chloride obtained in the step (1) into the reaction flask 2, heat up and stir, control the temperature in the reaction flask 2 to be 40°C, and add o-ethylaniline dropwise in the reaction flask 2, Among them, the molar ratio of ethyl oxalyl chloride to o-ethylaniline is 1.5:1. After the reaction, cool down to normal temperature, add 5% sodium carbona...

Embodiment 3

[0055] A preparation method for an ultraviolet absorber, comprising the steps of:

[0056] (1) the synthetic method of ethyl oxalyl chloride:

[0057]

[0058] Add oxalyl chloride in the reaction flask 1, control the temperature in the reaction flask to be 0°C, and add absolute ethanol dropwise to the reaction flask 1 under the condition of stirring, the molar ratio of the oxalyl chloride to the absolute ethanol is 1 : 1.5, after the reaction finished, rectification and purification obtained ethyl oxalyl chloride;

[0059] (2) Synthesis of oxalamide ester intermediate:

[0060]

[0061] Add the dichloroethane solvent and ethyl oxalyl chloride obtained in the step (1) into the reaction flask 2, heat up and stir, control the temperature in the reaction flask 2 to be 60°C, and add o-ethylaniline dropwise in the reaction flask 2, Among them, the molar ratio of ethyl oxalyl chloride to o-ethylaniline is 2:1. After the reaction, cool down to normal temperature, add 5% aqueou...

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Abstract

The invention relates to a preparation method for an ultraviolet absorbent. The preparation method comprises the following steps: (1) synthesis of an oxamate intermediate: with ethyl oxalyl chloride and o-ethylaniline as raw materials, dissolving the ethyl oxalyl chloride into a solvent, carrying out heating under stirring, dropwise adding the o-ethylaniline for a reaction, and after completion ofthe reaction, carrying out washing with water to remove the solvent so as to obtain the oxamate intermediate; (2) synthesis of an N-(2-ethoxyphenyl)-N'-(4-ethylphenyl)-oxalamide product: with o-phenetidine and the oxamate intermediate obtained in the step (1) as raw materials and Lewis base as a catalyst, heating the o-phenetidine, the oxamate intermediate and the Lewis base under stirring for areaction, after completion of the reaction, carrying out distillation at 120 to 170 DEG C to remove an ethanol by-product, carrying out cooling, pouring methanol, carrying out dissolving under stirring, carrying out filtering to remove an insoluble matter, cooling a mother liquor for crystallization, and carrying out filtering and drying so as to obtain a product. The preparation method provided by the invention has the advantages of simple technical process, low requirements on equipment, high product purity, high product yield, little three-wastes, facilitation of environmental protection, low production cost and applicability to industrial production.

Description

technical field [0001] The invention relates to a preparation method of an ultraviolet absorber, belonging to the technical field of ultraviolet absorber synthesis. Background technique [0002] Ultraviolet absorbers are the most widely used light stabilizers at present, which can absorb the ultraviolet rays in sunlight and fluorescent light sources without changing themselves. Because sunlight contains a large amount of ultraviolet light harmful to colored objects, its wavelength is about 290-460 nanometers, these harmful ultraviolet light through chemical oxidation and reduction, so that the color molecules finally decompose and fade, and the use of ultraviolet absorbers can prevent harmful ultraviolet rays. Ultraviolet light damages the color. [0003] N-(2-ethoxyphenyl)-N'-(4-ethylphenyl)-oxalamide is a new type of ultraviolet absorber, which has a very good absorption effect on ultraviolet rays, and is also more and more popular Welcomed by the industry, the current c...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/56
CPCC07C231/02C07C67/14C07C233/56C07C69/716
Inventor 张文庆张秀秀王轲
Owner 安徽新秀化学股份有限公司