Synthesis process of 4-amino antipyrine product and preparation method of synthesis process of 4-amino antipyrine product and preparation method

Abstract

The invention provides a synthesis process of 4-amino antipyrine product and a preparation method of a test solution for the process. The synthesis process comprises the following steps that antipyrine and 50% sulfuric acid are prepared into a solution, the solution and a sodium nitrite solution simultaneously flows into a nitrosation reactor, the flows of the solution and the sodium nitrite solution are controlled, the reaction temperature is controlled to be 45-50 DEG C, reaction is performed under stirring, a reaction terminal is tested by using an iodine powder starch test paper to adjust water flow, nitroso antipyrine generated through nitrosation instantly flows into a reduction tank to react with a reducing agent ammonium hydrogen sulfite and a water solution of ammonium sulfite which are prepared in the tank, a sample is taken to determine a pH value and the degree of reduction, the pH value ranges from 5.4 to 5.8, and the degree of reduction is 15. After reduction is completed, the pH value is regulated to be 5.8 to 6.0, the degree of reduction is about 5, the temperature is heated to reach 100 DEG C, hydrolysis is performed for 3 hours, cooling is performed to reach 80 DEG C, liquid ammonia is neutralized to reach pH of 7-7.5, and standing and layering are performed. The synthesis process is simple and easy to operate, and a preparation method is best in effect and has the advantages of being precision and rigorous.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a synthesis process of a 4-aminoantipyrine product and a method for preparing a test solution thereof. Background technique [0002] Antipyrine Chinese aliases: antipyrine, amtipyrine, 1,5-dimethyl-2-phenyl-3-pyrazolone, phenazone, dimethylphenylpyrazolone; Color crystal or white crystalline powder. Soluble in benzene, ethanol, water, chloroform, slightly soluble in ether; odorless, slightly bitter taste; solubility in water: 1000 g / l (20°C); mainly used as analytical reagent for nitric acid, nitrous acid and iodine. Determination of elements that can form complex cations (such as bismuth, tin, antimony and mercury, etc.). Gravimetric determination of titanium; colorless crystal or white crystalline powder, odorless, slightly bitter taste; easily soluble in water, ethanol, chloroform, slightly soluble in ether. It is mostly used in compound p...

AI Technical Summary

Problems solved by technology

But, the synthetic technique of existing 4-aminoantipyrine product and the preparation method thereof test solution have complex technique, inconvenient operation, poor effect of purification method, and lack of rigor. Therefore, a 4-aminoantipyrine is invented. The synthesis process of aminoantipyrine products and the preparation method of its test solution appear to be very necessary

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