A method for accelerating the synthesis time of mefenamic acid

A technology of mefenamic acid and its synthesis method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low product yield, long synthesis time, high production cost, etc., and achieve good product quality, Synthesis time is fast, the effect of speeding up the synthesis time

Active Publication Date: 2020-04-17
NINGBO SMART PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although several synthetic methods of mefenamic acid are disclosed in the art, there are always many weak points, such as higher production cost, longer synthesis time, and lower product yields

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add 57g of N,N-dimethylformamide, 150g of o-chlorobenzoic acid and 105g of sodium carbonate successively into the reactor equipped with a rectification column with theta ring as filler. After stirring for 10 minutes, start heating to raise the temperature, and when the internal temperature rises to 80° C., keep the reaction for 1 hour.

[0023] (2) Then add 230g of toluene (recovery toluene), heat it to reflux, the packing height of the packed tower is 20cm, the inner diameter of the packing is 3cm, and the insulation thickness is 0.5cm. Continue heating when the internal temperature reaches 112°C, start to drain water and keep the internal temperature at 100-120°C. When the displacement is 9ml, add 120g of 2,3-dimethylaniline after 1 hour with water in toluene and add 1.1g of copper powder when the internal temperature is 104°C without heating. After about 20 minutes, the reaction is intense and the liquid level After the reaction slows down, continue to heat up, ...

Embodiment 2

[0026] (1) Add 190kg N, N-dimethylformamide, 500kg o-chlorobenzoic acid and 350kg sodium carbonate successively in the reaction kettle equipped with the rectifying tower with the West tower ring as filler. After stirring for 10 minutes, start heating to raise the temperature, and when the internal temperature rises to 80° C., keep the reaction for 1 hour.

[0027] (2) then add 770kg of toluene (recovery toluene), heating it to reflux, the packing height of the packed tower is 500cm, the packing inner diameter is 80cm, and the insulation thickness is 11cm. Continue heating when the internal temperature reaches 112°C, start to drain water and keep the internal temperature at 100-120°C. When the displacement is ≤500mL, add 400kg of 2,3-dimethylaniline after 1.5 hours with water and add 3.5kg of copper powder when the internal temperature is 104°C without heating. After about 20 minutes, the reaction is intense and the liquid level After the reaction slows down, continue to heat ...

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Abstract

The invention relates to a method for accelerating synthetic time of mefenamic acid. The method comprises the following steps: performing a reaction by taking o-chlorobenzoic acid, sodium carbonate and 2,3-dimethyl aniline as main raw materials, taking copper powder as a catalyst, and taking N,N-dimethyl formamide and toluene as solvents, performing heating, enabling mixed steam in a reaction kettle to enter a rectifying tower which uses a Dixon ring as a filler, finally performing acidification, performing cooling, and performing filtering to obtain the mefenamic acid crude product. Accordingto the invention, drainage time in the reaction process is accelerated through continuous reflux and evaporation of the rectifying tower, so that the overall synthetic time of the mefenamic acid is accelerated, and the method has the advantages of a high reaction yield, good product quality and high synthetic time, reduces the costs, solves the problem of relatively long synthetic time in a current preparation method, and has good application prospects.

Description

technical field [0001] The invention belongs to the field of drug synthesis, in particular to a method for accelerating the synthesis time of mefenamic acid. Background technique [0002] Mefenamic acid is also known as mefenamic acid, paracetamol, etc., and its English name is Mefenamic Acid. It itself is an anti-inflammatory drug, mainly by inhibiting the synthesis of prostaglandins and proteolytic enzymes, thereby stabilizing the protein structure of the cell membrane and interfering with the tissue metabolic process. Clinically, it is often used to treat rheumatism, rheumatoid arthritis, dysmenorrhea, headache, neuralgia, muscle pain and other postoperative inflammatory pains. In addition, mefenamic acid can also be used as a precursor of acridine antimalarials and anticancer drugs. Just because mefenamic acid has such a broad application prospect, in recent years, various countries are studying and improving the synthesis process of mefenamic acid to increase economic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/08C07C227/18C07C227/40C07C229/58
Inventor 王闯
Owner NINGBO SMART PHARMA
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