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Preparation method of p-aminophenylacetic acid

A technology of p-aminophenylacetic acid and p-nitrophenylacetic acid, which is applied in the field of p-aminophenylacetic acid preparation, can solve the problems of difficult solid waste, low product yield, backward technology, etc., and achieve good purity, high yield, cost reduction effect

Active Publication Date: 2016-11-09
HEFEI PINGGUANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the process of preparing p-aminophenylacetic acid by reducing p-nitrophenylacetic acid is usually selected, mainly using iron powder as a reducing agent, but the method using iron powder as a reducing agent is cumbersome to operate, the process is backward, and the product yield is not high, and Can produce a large amount of solid waste that is difficult to handle, therefore, need to provide a kind of new preparation method of p-aminophenylacetic acid

Method used

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  • Preparation method of p-aminophenylacetic acid
  • Preparation method of p-aminophenylacetic acid

Examples

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Embodiment 1

[0022] A preparation method for p-aminophenylacetic acid, comprising the steps of: mixing water, ferric chloride, and p-nitrophenylacetic acid, heating up to 60°C under a nitrogen atmosphere, adding an aqueous solution of hydrazine hydrate dropwise, keeping the temperature for 2 hours, and cooling down to 20°C. ℃ to crystallize, filter to take the filter cake, wash with water, and dry to obtain p-aminophenylacetic acid, wherein the weight ratio of water, ferric chloride, p-nitrophenylacetic acid, and hydrazine hydrate is 10:0.05:1:0.45, wherein, for The amount of water used to wash the filter cake is not included.

Embodiment 2

[0024] A preparation method for p-aminophenylacetic acid, comprising the steps of: mixing water, ferric chloride, and p-nitrophenylacetic acid evenly, heating up to 90°C under a nitrogen atmosphere, adding an aqueous solution of hydrazine hydrate dropwise, keeping the temperature for 1 hour, and cooling down to 5 ℃ to crystallize, filter to take the filter cake, wash with water, and dry to obtain p-aminophenylacetic acid, wherein the weight ratio of water, ferric chloride, p-nitrophenylacetic acid, and hydrazine hydrate is 10:0.2:1:1, wherein, for The amount of water used to wash the filter cake is not included.

Embodiment 3

[0026] A preparation method for p-aminophenylacetic acid, comprising the steps of: mixing water, ferric chloride, and p-nitrophenylacetic acid, heating up to 70°C under a nitrogen atmosphere, adding hydrazine hydrate aqueous solution dropwise, keeping the temperature for 1.8h, and cooling down to Crystallize at 15°C, filter the filter cake, wash with water, and dry to obtain p-aminophenylacetic acid, wherein the weight ratio of water, ferric chloride, p-nitrophenylacetic acid, and hydrazine hydrate is 10:0.2:1:0.55, wherein, use The amount of water used to wash the filter cake is not included.

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Abstract

The invention discloses a preparation method of p-aminophenylacetic acid. The method comprises the following steps: uniformly mixing water, iron chloride and p-aminophenylacetic acid, heating the materials to the temperature of 60-90 DEG C under nitrogen atmosphere, dropping a hydrazine hydrate aqueous solution, insulating for 1-2 hours, cooling the material for crystallization, filtering the material to take a filter cake, washing the filter cake, and drying the product to obtain p-aminophenylacetic acid. According to the method, a difficulty processed solid waste is not generated, an organic solvent is not required, the environment is protected, the reaction condition is mild, operation is simple, and the method is suitable for industrial production, yield is high, the purity of the prepared p-aminophenylacetic acid is good, and the method provides the help for normal and stable production for actarit.

Description

technical field [0001] The invention relates to the technical field of p-aminophenylacetic acid preparation, in particular to a preparation method of p-aminophenylacetic acid. Background technique [0002] Actarit is a unique anti-rheumatic drug with low side effects and has advantages in the long-term treatment of rheumatoid arthritis, and can be used as a therapeutic drug for the initial stage of rheumatoid arthritis. At the same time, the combination of actarit and methotrexate can reduce the dosage of methotrexate and reduce adverse reactions. Actarit is a colorless needle crystal with the molecular formula C 10 h 11 NO 3 , CAS No. 18699-02-0, melting point 173-175°C, easily soluble in methanol, soluble in ethanol or anhydrous ether, slightly soluble in acetone, slightly soluble in water, very slightly soluble in ether. Its structural formula is as follows: [0003] [0004] The molecular formula for p-aminophenylacetic acid is C 8 h 9 NO 2 , CAS No. 1197-55-3...

Claims

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Application Information

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IPC IPC(8): C07C229/42C07C227/04
CPCC07C227/04C07C229/42
Inventor 王康林黄志生张成栋李海剑王高进
Owner HEFEI PINGGUANG PHARMA
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