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A kind of preparation method of acetaminophenacetic acid

A technology of p-aminophenylacetic acid and p-acetamido is applied in the field of preparation of p-acetamidophenylacetic acid, can solve the problems of cumbersome process operation, high cost of raw materials, low product yield and the like, achieves simplified operation steps, improved comprehensive yield, good purity

Active Publication Date: 2019-01-25
HEFEI PINGGUANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process operation is cumbersome, many times of filtration and drying are required in the preparation process, the cost of raw materials is relatively high, and the product yield is not high

Method used

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  • A kind of preparation method of acetaminophenacetic acid
  • A kind of preparation method of acetaminophenacetic acid

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Effect test

Embodiment 1

[0022] A preparation method of p-acetamidophenylacetic acid, comprising the following steps: mixing p-aminophenylacetic acid, N,N-dimethylacetamide, and ammonium chloride, heating to reflux, then cooling down to crystallize, and taking the crystals to obtain p-acetamido Phenylacetic acid.

Embodiment 2

[0024] A preparation method of para-acetaminophenylacetic acid, comprising the following steps: uniformly mixing p-aminophenylacetic acid, N,N-dimethylacetamide, and ammonium chloride, heating to 160°C, refluxing for 5h, cooling and crystallizing, and obtaining Crystallization obtains para-acetamidophenylacetic acid, wherein, the weight-to-volume (g / ml) ratio of p-aminophenylacetic acid and N,N-dimethylacetamide is 3:5, and the weight ratio of p-aminophenylacetic acid and ammonium chloride is 1:1.

Embodiment 3

[0026] A preparation method of p-acetaminophenylacetic acid, comprising the steps of: mixing p-aminophenylacetic acid, N,N-dimethylacetamide, and ammonium chloride, heating to 170°C, refluxing for 1h, and then cooling to room temperature, Add ice water to cool down and crystallize, filter, and dry to obtain p-aminophenylacetic acid, wherein the weight-to-volume (g / ml) ratio of p-aminophenylacetic acid and N,N-dimethylacetamide is 3:20, and p-aminophenylacetic acid 1. The weight ratio of ammonium chloride is 3:1, and the weight ratio of p-aminophenylacetic acid and ice water is 1:1 during the cooling crystallization process.

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Abstract

The invention discloses a method for preparing 4-acetylaminophenylacetic acid. The method includes the steps that p-nitrophenylacetic acid, N,N-dimethylacetamide and ammonium chloride are evenly mixed, heating reflux, cooling and crystallizing are conducted, and crystals are obtained to obtain 4-acetylaminophenylacetic acid. The production cost is low, the yield is high, product purity is good, operation is easy, the production period is short, and the method is suitable for industrial mass production.

Description

technical field [0001] The invention relates to the technical field of preparation of p-acetaminophenylacetic acid, in particular to a preparation method of p-acetaminophenylacetic acid. Background technique [0002] The chemical name of actarit is para-acetaminophenacetic acid, and its molecular formula is C 10 h 11 NO 3 , CAS No. 18699-02-0, melting point 173-175°C, colorless needle crystal, easily soluble in methanol, soluble in ethanol or anhydrous ether, slightly soluble in acetone, slightly soluble in water, very slightly soluble in ether. Actarit is a unique anti-rheumatic drug with low side effects and advantages in the long-term treatment of rheumatoid arthritis, and can be used as a treatment 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. Its structural formula is as follows: [0003] [0004] At present, the chemical synth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/10C07C233/54
CPCC07C231/10C07C233/54
Inventor 王康林黄志生张成栋汪祥
Owner HEFEI PINGGUANG PHARMA
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