Refining method for preparing high-purity oteracil potassium

A technology of potassium oxonate and a purification method, applied in directions such as organic chemistry, can solve the problems of not specifying product purity, not providing a purification method, etc., and achieving the effects of not easy side reactions and strong operability

Active Publication Date: 2010-10-20
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] EP0957096A1 provides a method, using allantoin as the starting material, converting the five-membered ring into a six-membered ring under the action of liquid bromine and KI, and then forming a salt in KOH aqueous solution to obtain potassium oxonate with a yield of 70 %, no refining method provided, nor product purity stated

Method used

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  • Refining method for preparing high-purity oteracil potassium
  • Refining method for preparing high-purity oteracil potassium
  • Refining method for preparing high-purity oteracil potassium

Examples

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Effect test

Embodiment 1

[0029] Add 10g of crude potassium oxonate to 90ml of water, add 10% potassium hydroxide solution under stirring until the crude product is completely dissolved, then add 8.5ml of acetone, stir at 25°C for half an hour, and adjust the pH to 6.9-7.2 with 10% hydrochloric acid while stirring , white crystals were precipitated, after the crystallization was completed, the filter cake was washed with acetone, and the filter cake was vacuum-dried, and weighed to obtain 9.2 g of high-purity potassium oxonate, with a yield of 92% and a purity of 99.98% (HPLC detection).

Embodiment 2

[0031] Add 10g of crude potassium oxonate potassium into 70ml of water, add 15% potassium carbonate solution under stirring until the crude product is completely dissolved, then add 7ml of methanol, stir at 10°C for half an hour, adjust the pH to 6.9-7.2 with 8% sulfuric acid while stirring, and White crystals were precipitated, and after the crystallization was completed, the filter cake was filtered, washed with methanol, dried in vacuum, and weighed to obtain 9.5 g of high-purity potassium oxonate, with a yield of 95% and a purity of 99.96% (HPLC detection).

Embodiment 3

[0033] Add 10g of crude potassium oxonate potassium to 100ml of water, add 10% potassium hydroxide solution under stirring until the crude product is completely dissolved, then add 10ml of ethanol, stir at 35°C for half an hour, adjust the pH to 6.9-7.2 with 15% formic acid while stirring, White crystals were precipitated, and after the crystallization was completed, the filter cake was filtered, washed with ethanol, dried in vacuum, and weighed to obtain 9.3 g of high-purity potassium oxonate, with a yield of 93% and a purity of 99.95% (HPLC detection).

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Abstract

The invention provides a method for refining high-purity potassium oxonate. The method is characterized by comprising the following steps: adding an potassium oxonate crude product into water; adding alkali into the water until the crude product is completely dissolved; adding a polar solvent into the solution; adjusting the pH of the solution to neutrality by acid; filtering and separating out crystal; and drying the crystal so as to obtain the high-purity potassium oxonate. The method has the advantages of simple operation, mild reaction condition, high yield, pure product and the like, andhas yield over 90 percent, purity over 99.95 percent (detected by HPLC), and a single impurity peak reduced from 0.5 percent to below 0.05 percent.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for refining the drug compound potassium oxonate. Background technique [0002] Potassium oxonate, also known as Oteracil Potassium, chemical name: 1,4,5,6-tetrahydro-4,6-dioxo-1,3,5-triazine- 2-Potassium carboxylate, the chemical structural formula is as follows: [0003] [0004] As one of the main components of a compound anticancer drug, fluterazine (TS-1), although it does not exhibit antitumor activity itself, it remains in the gastrointestinal tract and can inhibit 5-fluorouracil (5-FU) Activation at this position, thereby inhibiting the toxic and side effects of the antineoplastic drug tegafur, potassium oxonate can selectively act on orotate phosphoribosyltransferase in the gastrointestinal tract, block fluorouracil phosphorylation, reduce The resulting toxic and side effects of the gastrointestinal tract, potassium oxonate can also inhibit the reduction in fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/20
Inventor 赵志全张贵民
Owner LUNAN PHARMA GROUP CORPORATION
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