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Refining method of oteracil potassium

A technique for refining oteracil potassium, which is applied in the field of refining oteracil potassium, can solve the problems of easy decarboxylation, inability to remove impurities, increase of operation steps and production cost, and achieve stable quality, yield and purity Improved effect

Active Publication Date: 2012-10-24
NANJING CHIA TAI TIANQING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This shows that in the prior art, the purification of oteracil potassium, the refining method all adopts the processing method of "alkali-dissolved acid analysis", yet, in the "alkali-dissolved acid analysis" method operation process, the addition speed of acid and the The pH value of the solution is strictly controlled, thereby increasing the operation steps and production costs; in addition, oteracil potassium is easier to decarboxylate in acidic solution, and degrades into inactive metabolite 5-AZU, i.e. 1,3,5- Triazine-2,4(1H,3H)-dione, which is a by-product in the production process of oteracil potassium, is similar to the properties of oteracil potassium, and the method of "alkali dissolution and acid precipitation" is used for oteracil potassium When Tiracil Potassium is refined, when acid is added to the alkaline solution of Oteracil Potassium, the local acidity of the solution will be too strong in a short period of time, resulting in the decarboxylation of Oteracil Potassium to generate 5-AZU
Therefore, the traditional refining method of "alkali dissolution and acid precipitation" cannot remove the impurity stably and completely

Method used

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  • Refining method of oteracil potassium
  • Refining method of oteracil potassium
  • Refining method of oteracil potassium

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Adopt HPLC method to measure the purity of oteracil potassium among the present invention, chromatographic condition is as follows: stationary phase: octadecylsilane bonded silica gel; Mobile phase: phosphate buffer saline-methanol (9: 1), wherein phosphate buffer saline The composition of the solution is: potassium dihydrogen phosphate 0.65g, add water to 900mL, add 10% tetrabutylammonium hydroxide 2mL, adjust pH to 3.2 with phosphoric acid;

[0030] Column temperature: 35°C; detection wavelength: 220nm; injection volume: 10μL.

Embodiment 2

[0032] Add 1kg of crude product of oteracil potassium to 7.5L of aqueous solution containing 8% potassium carbonate, heat to 35°C, stir until the solid dissolves, filter, add 5L of ethanol to the filtrate, cool to 5°C, and stand for crystallization for 2 hours, filtered, and the filter cake was vacuum-dried at 60° C. to obtain 943 g of oteracil potassium crystals, with a yield of 94.3%. After HPLC detection, the peak time of 10.0 minutes is oteracil potassium, with a peak area of ​​99.9765%, and the peak time of 1.98 minutes is impurity 5-AZU, with a peak area of ​​0.0235%.

Embodiment 3

[0034] Add 1 kg of oteracil potassium crude product to 15 L of aqueous solution containing 1% triethylamine, heat to 50 ° C, stir until the solid dissolves, filter, add 18 L of ethanol and acetone mixed solution to the filtrate, cool to 5 ° C, Stand still for crystallization for 8 hours, filter, and vacuum-dry the filter cake at 60° C. to obtain 912 g of oteracil potassium crystals, with a yield of 91.2%. Through HPLC detection, the peak time of 10.0 minutes is oteracil potassium, with a peak area of ​​99.9680%, and the peak time of 1.98 minutes is impurity 5-AZU, with a peak area of ​​0.0320%.

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Abstract

The invention relates to the technical field of medicines and chemical industry, and specifically relates to a refining method of oteracil potassium. The refining method comprises the steps of heating and dissolving oteracil potassium crude product in aqueous solution containing alkaline matter, filtering, adding one or more of polar organic solvent to filtrate, cooling and crystallizing, and filtering to obtain high-purity oteracil. By adopting the refining method, oteracil potassium with the purity more than 99.96% can be obtained and the yield achieves more than 90%. The refining method has the advantages of being easy and simple to operate, low in production cost and high product purity, and is suitable for industrial production and use.

Description

technical field [0001] The invention relates to the technical field of medicine and chemical industry, in particular to a method for refining oteracil potassium. Background technique [0002] Potassium oxonate, also known as potassium oxonate, CAS registration number: 2207-75-2, chemical name: 1,4,5,6-tetrahydro-4,6-dihydro-1, 3,5-triazine-2-carboxylate potassium, the chemical structural formula is as follows: [0003] [0004] Oteracil Potassium is one of the main ingredients in the oral anti-cancer compound drug Sigio Capsules, developed by Japan Dapeng Pharmaceutical Co., Ltd., and approved for gastric cancer, non-small cell cancer, colon cancer, etc. The treatment of a variety of cancers, mainly composed of the active ingredient tegafur and two biochemical regulators gimeracil and oteracil potassium. [0005] Oteracil potassium itself does not have anti-tumor activity. After taking it, the drug stays in the gastrointestinal tract and selectively acts on orotate phos...

Claims

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Application Information

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IPC IPC(8): C07D251/20
Inventor 王华萍洪声柴雨柱徐丹杨治旻田舟山
Owner NANJING CHIA TAI TIANQING PHARMA
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