Synthetic process of 4-ampyrone product

A technology of aminoantipyrine and aminoantipyridine, which is applied in the field of medicine and chemical industry, can solve the problems of complex process, inconvenient operation, poor purification method effect and the like, and achieves the effects of simple process, convenient operation and high yield

Inactive Publication Date: 2017-05-24
湖州吴兴道场城乡建设发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is complex process in the synthetic technique of existing 4-aminoantipyrine product, inconvenient operation, the problem that purification method effect is poor,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A kind of synthesis technique of 4-aminoantipyrine product of the present invention, the steps are as follows:

[0016] 1) Make a solution of antipyrine and 50% sulfuric acid.

[0017] 2) Flow the solution and the sodium nitrite solution into the nitrosation reactor at the same time, control the flow of both, control the reaction temperature to 45-50°C, react under stirring, and measure the reaction end point with iodine powder starch test paper to adjust the water flow.

[0018] 3) The nitrosoantipyrine generated by nitrosation immediately flows into the reduction tank, and reacts with the aqueous reducing agent prepared in the tank.

[0019] 4) Take a sample to measure the pH value. When the pH value is between 5.4-5.8, the reduction is completed. Adjust the pH value to 5.8-6.0, heat up to 100°C, hydrolyze for 3 hours, cool down to 80°C, and neutralize with liquid ammonia to pH7-7.5 , standing layered.

[0020] 5) Separation of waste water to obtain 4-aminoantipyrin...

Embodiment 2

[0025] A kind of synthesis technique of 4-aminoantipyrine product of the present invention, the steps are as follows:

[0026] 1) Make a solution of antipyrine and 60% sulfuric acid.

[0027] 2) Flow the solution and the sodium nitrite solution into the nitrosation reactor at the same time, control the flow of both, control the reaction temperature to 45-50°C, react under stirring, and measure the reaction end point with iodine powder starch test paper to adjust the water flow.

[0028] 3) The nitrosoantipyrine generated by nitrosation immediately flows into the reduction tank, and reacts with the aqueous reducing agent prepared in the tank.

[0029] 4) Take a sample to measure the pH value. When the pH value is between 5.4-5.8, the reduction is completed. Adjust the pH value to 5.8-6.0, heat up to 98°C, hydrolyze for 3.5h, cool down to 82°C, and neutralize with liquid ammonia to pH7- 7.5, static stratification.

[0030] 5) Separation of waste water to obtain 4-aminoantipyri...

Embodiment 3

[0035] A kind of synthesis technique of 4-aminoantipyrine product of the present invention, the steps are as follows:

[0036] 1) Make a solution of antipyrine and 40% sulfuric acid.

[0037] 2) Flow the solution and the sodium nitrite solution into the nitrosation reactor at the same time, control the flow of both, control the reaction temperature to 45-50°C, react under stirring, and measure the reaction end point with iodine powder starch test paper to adjust the water flow.

[0038] 3) The nitrosoantipyrine generated by nitrosation immediately flows into the reduction tank, and reacts with the aqueous reducing agent prepared in the tank.

[0039] 4) Take a sample to measure the pH value. When the pH value is between 5.4-5.8, the reduction is completed. Adjust the pH value to 5.8-6.0, heat up to 99°C, hydrolyze for 2.5h, cool down to 85°C, and neutralize with liquid ammonia to pH7- 7.5, static stratification.

[0040] 5) Separation of waste water to obtain 4-aminoantipyri...

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Abstract

The invention provides a synthetic process of a 4-ampyrone product, which comprises the following steps of: preparing antipyrine and sulfuric acid with concentration of 40 to 60% into solution; enabling the solution and sodium nitrite solution to simultaneously flow into a nitrosation reactor, controlling flow rates of the solution and the sodium nitrite solution, and controlling a reaction temperature to be 45 to 50 DEG C; performing a reaction with stirring; testing a reaction endpoint by iodine powder and starch test paper to regulate a water flow rate; enabling nitroso antipyrine generated by nitrosation to immediately flow into a reducing pot to react with a reducing agent ammonium hydrogen sulfite prepared in the pot and aqueous solution of ammonium sulfite; carrying out sampling and measuring a pH value and a reduction degree; heating to a temperature of 90 to 100 DEG C; after hydrolysis, cooling to a temperature of 80 to 85 DEG C; neutralizing to pH of 7 to 7.5 by liquid ammonia; carrying out standing and layering. The process provided by the invention is simple, convenient to operate and high in yield.

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. Background technique [0002] At present, the Chinese aliases of antipyrine are: antipyrine, aminopyrine, 1,5-dimethyl-2-phenyl-3-pyrazolone, phenazone, dimethylphenylpyrazole Ketone; colored 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 preparations with oth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/46
CPCC07D231/46
Inventor 范沈杰
Owner 湖州吴兴道场城乡建设发展有限公司
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