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A kind of preparation method of ethyl p-aminobenzoate

A technology of ethyl aminobenzoate and p-nitrobenzoic acid, applied in the field of preparation of ethyl p-aminobenzoate, can solve the problems of unsuitable publicity and open student experiments, high raw material prices, difficult separation and the like, and achieves high cost performance and product quality. Good quality and short time effect

Active Publication Date: 2021-04-20
浙江优创材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned method, method (1) step is loaded down with trivial details, and raw material price is high, is unsuitable to publicize and set up student's experiment; salt, not easy to separate

Method used

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  • A kind of preparation method of ethyl p-aminobenzoate
  • A kind of preparation method of ethyl p-aminobenzoate
  • A kind of preparation method of ethyl p-aminobenzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A preparation method of ethyl p-aminobenzoate, comprising the steps of:

[0034] (1) p-Nitrobenzoic acid, ethanol, composite catalyst are dropped in the reactor;

[0035] (2) Reaction for 7 hours under reflux conditions to obtain ethyl p-aminobenzoate, intermediate p-aminobenzoic acid, and unreacted complete p-nitrobenzoic acid;

[0036] (3) The catalyst was filtered out, and the filtered catalyst was washed with ethanol at 50° C. and used for the next batch of reactions. ;

[0037] (4) excess ethanol is removed from the reaction solution, and the residue is dissolved in toluene to obtain a toluene reaction solution;

[0038] (5) the toluene reaction solution is washed with alkali and washed with water, and left to stand for stratification to obtain a toluene layer and an alkaline water layer;

[0039] (6) the toluene layer obtains ethyl p-aminobenzoate through cooling, crystallization, and centrifugation, and obtains the finished product of ethyl p-aminobenzoate aft...

Embodiment 2-6

[0047] Embodiment 2-6 (following embodiment is used for researching the impact of composite catalyst on product)

[0048] Others are all the same as in Example 1, except that the composite catalyst is different, and the details are as follows:

[0049] The influence of table 1 composite catalyst on product

[0050]

Embodiment 7-11

[0051] Embodiment 7-11 (following embodiment is used for researching the impact of composite catalyst preparation method on product)

[0052] Others are all the same as in Example 1, except that the preparation method of the composite catalyst is different, and the details are as follows:

[0053] Table 1 The impact of the composite catalyst preparation method on the product

[0054]

[0055]

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Abstract

The invention relates to the technical field of fine chemicals, in particular to a preparation method of ethyl p-aminobenzoate. A kind of preparation method of p-aminobenzoic acid ethyl ester of the present invention is characterized in that, comprises the following steps: (1) p-nitrobenzoic acid, ethanol, composite catalyst are dropped into reactor; (2) react 6- 8h, obtain ethyl p-aminobenzoate, intermediate p-aminobenzoic acid, and unreacted complete p-nitrobenzoic acid; (3) aftertreatment, obtain the finished product of p-aminobenzoic acid ethyl ester; the composite catalyst consists of sulfate , Inorganic reducing agent, diatomaceous earth, amine accelerator composition.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of ethyl p-aminobenzoate. Background technique [0002] Ethyl p-aminobenzoate is also known as benzocaine (ABEE). Colorless orthorhombic crystal, odorless and tasteless. Molecular weight 165.19. The melting point is 91-92°C. Soluble in alcohol, ether, chloroform. Soluble in almond oil, olive oil, dilute acid. Insoluble in water. It is clinically used for pain relief and antipruritic of wounds, ulcers, burns, skin abrasions and hemorrhoids. [0003] The synthetic route of benzocaine can be summarized as following 2 kinds: (1) take p-toluene gum as raw material, make benzocaine through acylation, oxidation, hydrolysis, esterification; Iron reduces p-nitrobenzoic acid to obtain p-aminobenzoic acid, and then esterifies with absolute ethanol under acidic conditions to obtain benzocaine. In the above-mentioned method, method (1) step is loaded down w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/60C07C227/04B01J31/26
CPCB01J31/26C07C227/04C07C2531/26C07C229/60
Inventor 茅月成吴建龙施根祥
Owner 浙江优创材料科技股份有限公司
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