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Preparation method of chemical intermediate benzocaine

A technology of benzocaine and carrier is applied in the preparation of chemical intermediate benzocaine and the field of chemical intermediate, and can solve the problems of poor color, low product yield, equipment corrosion and the like, and achieves high catalytic efficiency, The effect of reducing catalytic efficiency and high conversion rate

Inactive Publication Date: 2017-02-01
安徽金邦医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both methods have the problem of producing a large amount of waste acid, which not only pollutes the environment, but also easily corrodes the equipment, and the obtained product has problems such as low yield and poor color.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the preparation of benzocaine

[0024] Step S1, adding 4-nitrobenzoic acid, absolute ethanol, a solid catalyst and a water-carrying agent into a reaction vessel with a water separator, and refluxing for 3.5 hours; the solid catalyst uses magnesium aluminum hydrotalcite as a precursor, The modified nano-bentonite is used as a carrier, and the mass of the precursor is 35% of the mass of the carrier. The precursor and the carrier are ground and mixed uniformly, and then calcined at 600° C. for 3 hours to obtain the product;

[0025] Step S2, releasing the water in the water separator, adding absolute ethanol, and continuing to reflux and divide the water until no water drops appear;

[0026] Step S3, after the reaction is completed, filter while hot, and put the filtrate into a hydrogenation tank for hydrogenation reaction;

[0027] Step S4, after the hydrogenation is completed, after the system is heated to filter out the catalyst, it is filtered under the...

Embodiment 2

[0031] Embodiment 2: the preparation of benzocaine

[0032] Step S1, adding 4-nitrobenzoic acid, absolute ethanol, a solid catalyst and a water-carrying agent into a reaction vessel with a water separator, and refluxing for 1 hour; the solid catalyst uses magnesium aluminum hydrotalcite as a precursor, and the Nano-bentonite is used as the carrier, and the mass of the precursor is 25% of the mass of the carrier. The precursor and the carrier are ground and mixed uniformly, and then calcined at 500 ° C for 4 hours to obtain the product;

[0033] Step S2, releasing the water in the water separator, adding absolute ethanol, and continuing to reflux and divide the water until no water drops appear;

[0034] Step S3, after the reaction is completed, filter while hot, and put the filtrate into a hydrogenation tank for hydrogenation reaction;

[0035] Step S4, after the hydrogenation is completed, after the system is heated to filter out the catalyst, it is filtered under the prot...

Embodiment 3

[0039] Embodiment 3: the preparation of benzocaine

[0040] Step S1, adding 4-nitrobenzoic acid, absolute ethanol, solid catalyst and water-carrying agent into a reaction vessel with a water separator, and heating under reflux for 6 hours; the solid catalyst uses magnesium aluminum hydrotalcite as a precursor, and changes Nano-bentonite is used as the carrier, and the mass of the precursor is 45% of the mass of the carrier. The precursor and the carrier are ground and mixed evenly, and then calcined at 700 ° C for 2 hours to obtain the product;

[0041] Step S2, releasing the water in the water separator, adding absolute ethanol, and continuing to reflux and divide the water until no water drops appear;

[0042] Step S3, after the reaction is completed, filter while hot, and put the filtrate into a hydrogenation tank for hydrogenation reaction;

[0043] Step S4, after the hydrogenation is completed, after the system is heated to filter out the catalyst, it is filtered under...

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PUM

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Abstract

The invention discloses a preparation method of chemical intermediate benzocaine. The preparation method of the chemical intermediate benzocaine comprises the steps: S1, adding 4-nitrobenzoic acid, absolute ethanol, a solid catalyst and a water-carrying agent into a reaction container with a water segregator and performing hot reflux for 1 to 6 hours, wherein the solid catalyst takes magnesium aluminum hydrotalcite as a precursor and modified nanometer bentonite as a carrier, the weight of the precursor is 25 to 45 percent that of the carrier, and the solid catalyst is prepared by grinding and mixing the precursor and the carrier uniformly and calcining at 500 to 700 DEG C for 2 to 4 hours; S2, discharging water out of the water segregator, replenishing the absolute ethanol and continuously performing reflux and water segregation until no water drops occur; S3, after the reaction is finished, filtering when the reaction liquid is hot and putting the filtrate into a hydrogenation kettle to perform hydrogenation reaction; S4, after the hydrogenation is finished, performing heat filtration to remove the catalyst from the system, cooling and filtering under the protection of nitrogen, and drying to obtain the chemical intermediate benzocaine. The preparation method of the benzocaine, provided by the invention, is high in conversion rate; the solid catalyst has high catalytic efficiency and can be repeatedly used, and the catalytic efficiency is not obviously reduced after the catalyst is repeatedly used for 50 times.

Description

technical field [0001] The invention belongs to the field of chemical industry, relates to chemical intermediates, in particular to a preparation method of chemical intermediate benzocaine. Background technique [0002] Benzocaine is a kind of important chemical intermediate, mainly contains two kinds of synthetic methods at present: a kind of method is to take p-nitrobenzoic acid as raw material, take concentrated sulfuric acid or cationic exchange resin as catalyst and dehydrating agent, carry out with ethanol The esterification reaction obtains ethyl p-nitrobenzoate, and then obtains benzocaine through iron powder reduction; another method is to use ethyl p-aminobenzoate as raw material, using thionyl chloride, phosphorus oxychloride and Concentrated sulfuric acid is esterified with ethanol to obtain benzocaine. Both methods have the problem of producing a large amount of waste acid, which not only pollutes the environment, but also easily corrodes the equipment, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/12C07C229/60B01J21/10
CPCC07C227/12B01J21/10B01J23/007C07C229/60
Inventor 曹金龙
Owner 安徽金邦医药化工有限公司
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