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Environment-friendly method for preparing phenylbutazone

A kind of phenylbutazone, green technology, applied in the field of medicine and chemical industry, can solve the problems of inadequate control, incomplete reaction, too long reaction time, etc., to achieve the effect of reducing raw material cost, stable yield and qualified purity

Active Publication Date: 2018-07-13
JINGHUA PHARMA GRP NANTONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of waste water is produced in this process, and because the reaction is not properly controlled, the reaction is not complete or the reaction time is too long to produce impurities, resulting in a large amount of old oil residue during post-treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 80g of sodium methoxide methanol solution into a dry and clean 500mL four-neck flask, distill to dryness, add 68.8g of diethyl n-butylmalonate, stir until the sodium methoxide is completely dissolved, add 50g of hydroazobenzene, heat up, Control the internal temperature at 130°C, react for 3-4 hours, and take samples for HPLC control. If the relative content of hydroazobenzene is ≤0.5%, the reaction is complete. Recover A and ethanol until no alcohol is evaporated, add 250g of 95% ethanol to dissolve, then transfer to a 1L four-necked bottle, cool down to below 20°C and slowly add ethanol solution of hydrochloric acid (mixed solution of 150g of ethanol and 45g of 36% hydrochloric acid) Adjust the pH to 6, a large amount of white solids are precipitated, heated in a water bath to 65°C, the solids are completely dissolved, decolorized once with activated carbon, the decolorization time is 15min, filtered while it is hot, cooled to 0-5°C to crystallize, and obtained cru...

Embodiment 2

[0018] Add 80g of sodium methoxide methanol solution into a dry and clean 500mL four-neck flask, distill to dryness, add 68.8g of diethyl n-butylmalonate, stir until the sodium methoxide is completely dissolved, add 50g of hydroazobenzene, heat up, Control the internal temperature at 130°C, react for 3-4 hours, and take samples for HPLC control. If the relative content of hydroazobenzene is ≤0.5%, the reaction is complete. Recover methanol and ethanol until no alcohol is evaporated, add 200g of methanol and ethanol mixed solution (methanol content 18.7%) to dissolve, transfer it to a 1L four-necked bottle, cool down to below 20°C and slowly add hydrochloric acid solution of methanol and ethanol (70g of methanol, Ethanol and 45g of 36% hydrochloric acid mixed solution) to adjust the pH to 6, a large amount of white solids precipitated, heated to 65°C in a water bath, the solids were completely dissolved, decolorized once with activated carbon, the decolorization time was 15min, ...

Embodiment 3

[0020] Add 80g of sodium methoxide methanol solution into a dry and clean 500mL four-neck flask, distill to dryness, add 68.8g of diethyl n-butylmalonate, stir until the sodium methoxide is completely dissolved, add 50g of hydroazobenzene, heat up, Control the internal temperature at 130°C, react for 3-4 hours, and take samples for HPLC control. If the relative content of hydroazobenzene is ≤0.5%, the reaction is complete. Recover formazan and ethanol until no alcohol is evaporated, add 200g of recovered formazan and ethanol to dissolve, transfer to a 1L four-necked bottle, cool down to below 20°C and slowly add hydrochloric acid formazan and ethanol solution dropwise (70g recovered formazan, ethanol and 45g 36% hydrochloric acid mixed solution) to adjust the pH to 6, a large amount of white solids were precipitated, heated in a water bath to 65°C, the solids were completely dissolved, decolorized once with activated carbon, the decolorization time was 15min, filtered while it ...

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Abstract

The invention relates to an environment-friendly method for preparing phenylbutazone. A preparation method comprises the following steps: 1), distilling a methanol solution of sodium methoxide till dryness, then adding diethyl n-butylmalonate and hydrogenated azobenzene for reaction, and performing centralized control on the reaction; 2), recycling methanol and ethanol till dryness, then adding ethanol or mixed liquid of the recycled methanol and ethanol, and dissolving; 3), adjusting the pH with acid, separating out solid, dissolving the solid by heating in a water bath, decolorizing, thermally filtering, then cooling down for crystallizing, and performing suction filtration to obtain crude phenylbutazone and mother liquor; 4), heating the mother liquor, concentrating under reduced pressure, recycling ethanol, and refining the crude phenylbutazone with the ethanol to obtain refined phenylbutazone. The method has the advantages as follows: the centralized control is performed on the reaction by utilizing a liquid chromatograph, and water is replaced with the ethanol or the recycled methanol and ethanol as a solvent, so that the organic solvent can be recycled while the wastewater treatment cost is reduced; glacial acetic acid is replaced with hydrochloric acid as neutralizing acid, so that the raw material cost is reduced; therefore, the method is an environment-friendly chemical synthesis method with relatively good popularization and application prospects.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, and in particular relates to a green method for preparing phenylbutazone. Background technique [0002] Butazone is mainly used for the treatment of rheumatoid arthritis, rheumatoid arthritis, gout, and acute lymphangitis of filariasis, and it often needs to be administered continuously or used in combination with other drugs. The effect is similar to aminopyrine, but the anti-inflammatory effect is weaker, and the effect on inflammatory pain is better. It can promote the excretion of uric acid. The incidence of adverse reactions of this product is about 10%-20%. Such as short-term use of adverse reactions less. [0003] At present, the preparation method of phenylbutazone is: after reacting diethyl n-butylmalonate and hydrazobenzene under the catalysis of sodium methylate for 3 hours, reclaim formazan and ethanol to dryness, then add a large amount of water to dissolve,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/34
CPCC07D231/34
Inventor 沈小娟顾健波吴竞滕飞陈雪莲
Owner JINGHUA PHARMA GRP NANTONG