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Separation and purification process of diantipyrylmethane monohydrate

A technology of diantipyrine methane and process, which is applied in the field of separation and purification of diantipyrine methane, can solve problems affecting material quality, removal, and product crystallization rate, etc., and achieves the goal of improving economic benefits and simple process Effect

Active Publication Date: 2014-03-19
SHANDONG XINHUA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because diantipyrine methane is insoluble in water, the AA process, FAA process, and MAA process of Analgin production all use water as a solvent, which cannot be removed in the previous process and is brought into the finished product; and because diantipyrine Methane dissolves in concentrated ethanol, which affects both the quality of the material and the crystallization rate of the product in the last process of Analgin

Method used

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  • Separation and purification process of diantipyrylmethane monohydrate

Examples

Experimental program
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Effect test

Embodiment 1

[0023] After concentration, take 5000g of Sulpyrine and add 150g of water to filter at 65°C, filter out diantipyrine methane to obtain 521g of filter residue, add 521g of water, heat up to 70°C, keep warm for 1 hour, filter, and use 400g of water to Washed three times and dried to obtain 514g of solid material. Add 514g of ethanol and 10g of activated carbon to 514g of solid material, insulate at 70°C for 1 hour, cool down to 15°C, centrifuge, wash with 272g of water and 205g of ethanol, and spin dry to obtain 409g of solid material. Add 409 g of ethanol and 10 g of activated carbon to 409 g of solid material, insulate at 80 ° C for 1 hour, cool to 15 ° C, centrifuge, wash with 176 g of water and 156 g of ethanol, and spin dry to obtain 327 g of solid material. Dry at 60°C for 1 hour to obtain 294 g of dry product with a content of 99.2%.

Embodiment 2

[0025] Take 5000g of Sulpyrine after concentration and add 1000g of water to filter at 80°C, filter out diantipyrine methane to obtain 503g of filter residue, add 503g of water, heat up to 80°C, keep warm for 0.5 hours, filter, and pass through with 400g of water Washed three times and dried to obtain 497g of solid material. Add 497g of ethanol and 20g of activated carbon to 497g of solid material, keep warm at 75°C for 1 hour, cool down to 15°C, centrifuge, wash with 248g of water and 160g of ethanol, and spin dry to obtain 384g of solid material. Add 384g of ethanol and 15g of activated carbon to 384g of solid material, keep warm at 70°C for 1 hour, cool down to 15°C, centrifuge, wash with 192g of water and 172g of ethanol, and spin dry to obtain 305g of solid material. Dry at 80°C for 1.5 hours to obtain 278g of dry product with a content of 99.4%.

Embodiment 3

[0027] Take 5000 g of Sulpyrine Sperm after concentration and add 150 g of water to filter at 70° C., filter out diantipyrine methane to obtain 517 g of filter residue. Add 517g of water, heat up to 75°C, keep warm for 1.5 hours, filter, wash with 400g of water three times, and spin dry to obtain 503g of solid material. Add 503 g of ethanol and 15 g of activated carbon to 503 g of solid material, insulate at 80 ° C for 1 hour, cool to 15 ° C, centrifuge, wash with 251 g of water and 226 g of ethanol, and spin dry to obtain 383 g of solid material. Add 383g of ethanol and 15g of activated carbon to 383g of solid material, insulate at 75°C for 1 hour, cool to 15°C, centrifuge, wash with 190g of water and 172g of ethanol, and spin dry to obtain 302g of solid material. Dry at 70°C for 2 hours to obtain 272 g of dry product with a content of 99.3%.

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Abstract

The invention belongs to the pharmaceutical chemical field, and specifically relates to a separation and purification process of diantipyrylmethane monohydrate. The process comprises the following steps: adding water to the refined mother liquor of analgin, filtering, refining the filter residue with water, refining with ethanol, decoloring with active carbon, washing with water and ethanol, and drying to obtain the diantipyrylmethane monohydrate. The separation and purification process of diantipyrylmethane monohydrate is simple, scientific and rational in process; the diantipyrylmethane monohydrate is purified and separated so as to be sold as a byproduct; therefore, the economic benefit is improved.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a separation and purification process of diantipyrine methane. Background technique [0002] With the improvement of drug production quality in recent years, the Chinese Pharmacopoeia, European Pharmacopoeia, etc. have further increased the quality requirements for Analgin, and the requirements for impurities in the raw material drug Analgin have been further increased, and the original production of Analgin cannot meet the requirements of the Pharmacopoeia. , cannot leave the factory as a qualified product. The main task of the production of Analgin is to study the cause of the formation of Analgin impurities. [0003] Analgin is produced as antipyrine during the AT methylation stage, and studies have found that diantipyrine methane will be generated due to the AT methylation stage. Because diantipyrine methane is insoluble in water, the AA process, FA...

Claims

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Application Information

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IPC IPC(8): C07D231/26
CPCC07D231/26
Inventor 王凯广未雅楠方毅
Owner SHANDONG XINHUA PHARMA