Preparation method of N-(4-ethoxycarbonylphenyl)-N'-ethyl-N'-phenylformamidine

A technology of ethoxycarbonyl phenyl and phenylformamidine, which is applied in the field of preparation of N--N'-ethyl-N'-phenylformamidine, and can solve the problems of limiting large-scale industrial production, color and purity. , separation and purification are cumbersome and other problems, to achieve the effect of reducing energy consumption and labor intensity, product color is good, saving labor

Active Publication Date: 2010-09-22
遵义市倍缘化工有限责任公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

The disadvantage of this synthetic method is that the reaction process will be carried out at about 230°C at a higher temperature, and the intermediate will be taken out, and the high temperature reaction will cause the product N-(4-ethoxycarbonylphenyl)-N The color and purity of '-ethyl-N'-phenylformamidine are affected, and large-scale industrial production is limited
[0005] 2) Use N-phenyl-N-ethylformamide and ethyl p-aminobenzoate to synthesize N-(4-ethoxycarbonylphenyl)-N'-ethy

Method used

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  • Preparation method of N-(4-ethoxycarbonylphenyl)-N'-ethyl-N'-phenylformamidine

Examples

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Comparison scheme
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Embodiment 1

[0020] Put 150 kilograms of ethyl p-aminobenzoate, 270 kilograms of triethyl orthoformate and 150 kilograms of N-ethylaniline into a 1000-liter reactor with a separation tower, start stirring and heat up. When the temperature rises to 100°C, ethanol is generated, and the temperature is raised slowly to control the temperature at the top of the tower to be less than 78°C. When the ethanol is received to 110 liters, the temperature of the kettle is about 110-140°C. Keep it warm for 3 hours to recover triethyl orthoformate For ester, N-ethylaniline is recovered by distillation under reduced pressure. The temperature is controlled at 160°C. After the reaction is completed, it is moved to a 500-liter distillation pot for distillation. After removing the fore distillation, collect the fraction at 222-228°C / 1mmHg to obtain 250 kg of distillate. Then add 250 kilograms of distillate into a 1000-liter reaction kettle with 500 kilograms of methyl alcohol and stir to freeze and crystalliz...

Embodiment 2

[0022] Put 150 kilograms of ethyl p-aminobenzoate, 350 kilograms of triethyl orthoformate and 170 kilograms of N-ethylaniline into a 1000-liter reactor with a separation tower, start stirring and heat up. When the temperature rises to 100°C, ethanol is generated, and the temperature is raised slowly to control the temperature at the top of the tower to be less than 78°C. When the ethanol is received to 120 liters, the temperature of the kettle is about 110-140°C. Keep it warm for 3 hours to recover triethyl orthoformate For ester, N-ethylaniline is recovered by distillation under reduced pressure. The temperature is controlled at 160°C. After the reaction is completed, it is moved to a 500-liter distillation pot for distillation. After the fore distillation was removed, the fraction at 222-228°C / 1mmHg was collected to obtain 258 kg of distillate. Add 258 kilograms of distillate to 510 kilograms of methyl alcohol and freeze and crystallize in a 1000-liter reactor with stirring....

Embodiment 3

[0024] Put 150 kilograms of ethyl p-aminobenzoate, 270 kilograms of trimethyl orthoformate and 160 kilograms of N-ethylaniline into a 1000-liter reactor with a separation tower, start stirring and heat up. When the temperature rises to 80°C, methanol is produced, and the temperature is raised slowly to control the temperature at the top of the tower to be less than 68°C. When the methanol is received to 110 liters, the temperature of the kettle is about 110-140°C. Keep it warm for 3 hours to recover trimethyl orthoformate For ester, N-ethylaniline is recovered by distillation under reduced pressure. The temperature is controlled at 160°C. After the reaction is completed, it is moved to a 500-liter distillation pot for distillation. After the fore distillation was removed, the fraction at 222-228°C / 1mmHg was collected to obtain 256 kg of distillate. Add 256 kilograms of distillate to 500 kilograms of methyl alcohol and freeze crystallization in a 1000-liter reactor with stirrin...

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Abstract

The invention relates to a preparation method of N-(4-ethoxycarbonylphenyl)-N'-ethyl-N'-phenylformamidine, comprising the following steps of: simultaneously adding raw materials which are para-amino ethyl benzoate, tri-alkyl ortho-formate and N-ethylphenylamine into a reaction kettle, mixing and performing one-step condensation in the reaction kettle at 80 to 160 DEG C; distilling a reaction liquid under reduced pressure to produce a distilled product of the N-(4-ethoxycarbonylphenyl)-N'-ethyl- N'-phenylformamidine and then refining with alcohol to produce a finished product of the N-(4-ethoxycarbonylphenyl)-N'-ethyl- N'-phenylformamidine. The method lowers the reaction temperature, reduces the reaction step, improves the purity of product, reduces the pollution and equipment investment, saves labor and reduces energy consumption and labor intensity, has good product color, high content, low cost and simple operation, and is easy to realize large-scale industrial production.

Description

Technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of N-(4-ethoxycarbonylphenyl)-N'-ethyl-N'-phenylformamidine. Background technique [0002] N-(4-ethoxycarbonylphenyl)-N'-ethyl-N'-phenylformamidine is an efficient anti-ultraviolet additive, which can absorb ultraviolet light in the 240-300nm band, almost completely absorbing 300~ Ultraviolet rays in the 330nm band. Adding this absorbent in the production process of various organic materials such as plastic products, resin products, dyes, and textiles can reduce and avoid damage to the physical properties of the above-mentioned products due to the photodegradation of ultraviolet rays (such as product discoloration, decolorization or easy brittle, brittle). And compared with the UV absorbers of benzophenones or benzotriazoles, the UV resistance of N-(4-ethoxycarbonylphenyl)-N'-ethyl-N'-phenylformamidine More superior, better stability than N-(4-ethox...

Claims

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Application Information

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IPC IPC(8): C07C257/12
Inventor 胡敬蒋生庚张基明蒋家均
Owner 遵义市倍缘化工有限责任公司
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