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
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[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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