Synthesis and fine purification method of flunixin meglumine

A technology of flunixin meglumine and its refining method, which is applied in the direction of organic chemistry, can solve the problems of high production cost and long process flow, and achieve the effects of simple operation, high yield and easy implementation

Inactive Publication Date: 2006-07-19
SHANDONG LUKANG SHELILE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the prior art, for the elimination reaction between the halide and the amino compound with a shuttle group, generally speaking, the shuttle group must be protect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0018] Embodiment (1): First, add 280 grams of 2-methyl-3-(trifluoromethyl)aniline, 126.5 grams of 2-chloronicotinic acid, and 350 milliliters of water into a 1000 milliliter reaction flask with a condenser tube and a stirrer and 12 grams of p-toluenesulfonic acid-hydrate, the heating temperature was controlled at 98-105°C under stirring and kept for 20 hours. Stop heating and lower the temperature below 80°C, add dropwise 20% potassium hydroxide solution to the reaction solution until the pH value reaches above 11.5, continue to stir and cool down to below 30°C, and obtain incompletely reacted 2-methyl- 110 grams of 3-(trifluoromethyl)aniline (can be used in the future); about 500 milliliters of brown-red synthetic extract.

[0019] Example (2): The synthetic extract is decolorized and filtered, and concentrated sulfuric acid crystals are added dropwise until the pH value is about 4.5. After filtering, the filter cake is dried, dissolved in methanol, filtered, cooled and sta...

Embodiment ( 4

[0021] Embodiment (four): 100 grams of flunixin meglumine salt (2-[[2-methyl 3-(trifluoromethyl) phenyl] amino] the meglumine salt of nicotinic acid) crude product is dissolved in 800 ml of water, after filtering, put it into a 2000 ml stirred reaction bottle, heat in a water bath and concentrate under negative pressure, stop heating when the color of the concentrated liquid becomes dark, add sperm and continue stirring while cooling down, when a large number of sperm nuclei are produced, stop stirring , continue to cool down to below 20 degrees, filter and dry to obtain 80 grams of flunixin meglumine salt finished product. The quality is in full compliance with the fifth edition of the European Pharmacopoeia.

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Abstract

The synthesis and extraction and refine method for meglumine flunixin comprises: with p-toluenesulfonic monohydrate as catalyst and 20% KOH as extract, selecting 2-methyl-3- (trifluoromethyl) aniline and 2-chloronicotioyl by mole ratio as 2:1 for reaction with end pH value more than 11.5; cooling and crystallizing the residual aniline to separate and recover; using methanol in extraction and purification for flunixin; static cooling and crystallizing, and separating and cleaning the crystal to obtain the refined product; finally, recrystallizing to prepare the flunixin methylglucamine in water. This invention has high yield.

Description

Technical field: [0001] The invention relates to a method for synthesizing flunixin meglumine salt with 2-methyl-3-(trifluoromethyl)aniline, 2-chloronicotinic acid and meglumine, especially the synthesis and extraction of flunixin meglumine Refining method. Background technique: [0002] In the prior art, for the elimination reaction between the halide and the amino compound with a shuttle group, generally speaking, the shuttle group must be protected, and the small molecule product generated is tried to be removed in the reaction process, but the process of using this technology The process is long and the production cost is high. Invention content: [0003] The object of the invention is to overcome the deficiencies of the prior art and provide a method for the synthesis, extraction and purification of flunixin meglumine, which adopts the feeding capacity of increasing 2-methyl-3-(trifluoromethyl)aniline And select suitable catalyst and suitable temperature of reaction...

Claims

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Application Information

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IPC IPC(8): C07D213/80C07D213/803
Inventor 袁洪斌吴娜王清江
Owner SHANDONG LUKANG SHELILE PHARMA
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