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Technology for preparing metamizole magnesium through one-pot method

A kind of technology of analgin magnesium and process, applied in the field of medicine, can solve the problems of high price of ion exchange resin, unstable product quality, unstable magnesium analgin, etc., and achieve the effects of stable process, high yield and simple process

Active Publication Date: 2019-08-27
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this method is that the ion exchange resin is expensive, and analgin magnesium is also unstable in aqueous solution, resulting in unstable product quality and higher production costs

Method used

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  • Technology for preparing metamizole magnesium through one-pot method
  • Technology for preparing metamizole magnesium through one-pot method
  • Technology for preparing metamizole magnesium through one-pot method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Add compound 4-methylaminoantipyrine (MAA) (217.3g, 1mol), MgO (40.3g, 1mol) formaldehyde solution (110g, mass fraction 36%) and 550ml methanol into a 1L reaction flask, 20-30 Stir at ℃ to disperse the system, slowly introduce SO 2gas, the reaction temperature is 30-80°C, and the end point of the reaction is judged by PH test paper in the later stage of aeration. And keep stirring at 20~50℃ for 1h. Lower the temperature of the reaction system to 0-25°C, heat and crystallize for 2 hours, then filter with suction, rinse the filter cake with a small amount of ice isopropanol, and dry it by blasting to obtain 350.2 g of analgin magnesium (ANJ-Mg), with a yield of 93% .

Embodiment 2

[0052] Compound MMA (217.3g, 1mol), MgO (40.3g, 1mol), formaldehyde solution (110g, mass fraction 36%) and 550ml isopropanol are added in the 1L reaction flask, and lead to sulfur dioxide in the reaction flask, the reaction temperature The temperature is 30-80° C., and the purity of MAA in the reaction system monitored by HPLC is less than or equal to 0.5%, which means the end of the reaction is judged. The reaction solution was cooled to 0-5°C in an ice-water bath and kept warm for crystallization for 2 hours, filtered with suction, washed the filter cake with a small amount of ice isopropanol, and dried by blasting to obtain 354.0 g of analgin magnesium, with a yield of 94%.

Embodiment 3

[0054] The compound MMA (217.3g, 1mol), MgO (40.3g, 1mol), formaldehyde solution (110g, mass fraction 36%) and 550ml of ethanol were added to a 1L reaction flask, and sulfur dioxide was introduced into the reaction flask, and the pressure was increased to the reaction flask. The internal pressure of the bottle is 40-60psi, and it is heated to 40-80°C to react. If the pressure of the reaction bottle drops, continue to pass sulfur dioxide to maintain the internal pressure of the reaction bottle at 20-50 psi. React until the internal pressure of the reaction bottle remains basically unchanged within 0.5 to 1 hour, then cool down to room temperature, cool the reaction solution to 0 to 5°C in an ice-water bath and keep it warm for crystallization for 2 hours, filter with suction, rinse the filter cake with a small amount of ice ethanol, and After air-drying, 338.9 g of analgin magnesium was obtained, with a yield of 90%.

[0055] Table 1: Effect of solvent type and dosage on the y...

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Abstract

The invention discloses a technology for preparing metamizole magnesium through a one-pot method. According to the one-pot method, 4-methylamino antipyrine, formaldehyde and magnesium salt or oxide ofthe magnesium salt are taken as raw materials and react with SO2 gas to prepare a 1-phenyl-2,3-dimethyl-4-methylamino pyrazoline-5-ketone-N-methanesulfonic acid magnesium crude product, the above crude product is recrystallized for further refining, and a 1-phenyl-2,3-dimethyl-4-methylamino pyrazoline-5-ketone-N-methanesulfonic acid magnesium hexahydrate is prepared. According to the technology,the steps are simple, the raw materials are cheap and easy to obtain, the synthesized metamizole magnesium finished product is high in yield and good in quality, and the technology is stable and suitable for industrial production.

Description

technical field [0001] The present invention relates to the field of medicine, specifically, the present invention relates to a kind of 1-phenyl-2,3-dimethyl-4-methylaminopyrazolin-5-one-N-methylsulfonic acid magnesium hexahydrate The preparation method and refining method. Background technique [0002] Analgin magnesium (1-phenyl-2,3-dimethyl-4-methylaminopyrazolin-5-one-N-methylsulfonate magnesium hexahydrate), can be used for emergency relief in acute high fever It can also be used for headache, migraine, muscle pain, rheumatic neuralgia, toothache, joint pain and menstrual pain; it can also be used as veterinary medicine for muscle pain, rheumatism, febrile disease and colic, etc. Its structure is simplified as follows: [0003] [0004] Through comprehensive literature research, we found that there are mainly two methods for preparing Analgin magnesium: [0005] Method 1: Patent CN99120402.6 reports the synthesis of Sulpyrine Magnesium by replacing Sulpyrine with ...

Claims

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Application Information

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IPC IPC(8): C07D231/48
CPCC07D231/48
Inventor 赵涛涛葛德芳张伟洪健艾娇皮金红张琦谢国范吴鸣
Owner WUHAN WUYAO PHARMA
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