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Method for preparing potassium oxonate

A technology of oteracil potassium and potassium iodide, which is applied in the field of chemical synthesis, can solve the problems of non-compliance with medicinal requirements, low product purity, high production cost, etc., and achieve the effects of favorable reaction, high product yield and low cost

Inactive Publication Date: 2016-11-09
山东川成医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method prepares oteracil potassium yield and only has about 50%, and yield is lower, and purity 98%, product purity is low, does not meet medicinal requirement, needs to be refined, just can obtain medicinal oteracil potassium, resulting in higher production costs

Method used

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  • Method for preparing potassium oxonate

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Dissolve 3.2Kg of potassium hydroxide in 11.4L of water, add it into a 20L reaction kettle, cool down to 0-5°C, add 46g of potassium iodide, add 0.9kg of allantoin in batches, stir to dissolve, and control the temperature at 0-5°C It takes 9 hours to add 1.8kg of bromine dropwise (according to the different bromine dropping time, they are respectively regarded as the 1-8 group). Bursulin figure 1

[0026] group

[0027] . figure 1 It is the relationship diagram between reaction temperature and yield in the embodiment of the present invention. Depend on figure 1 As can be seen, along with the increase of the bromine dripping time, the yield of oteracil potassium increases, and when the bromine dripping time is 9 hours, the yield can increase to 75.2%, and then prolong the dripping time later, the yield increases Not obvious.

Embodiment 2

[0029] Dissolve 3.2Kg of potassium hydroxide in 12.8L of water, add it into a 20L reaction kettle, cool down to 0-5°C, add 48g of potassium iodide, add 1.0kg of allantoin in batches, stir to dissolve, and control the temperature at 0-5°C It takes 9 hours to add 2.0kg bromine dropwise. After the dropwise addition, stir at 0-5°C for 1 hour, raise the temperature to 20-25°C and react for 20 hours. HPLC detects that allantoin is <0.6%, cool down to 0-5°C, and add acetic acid dropwise to adjust pH to 5, filtered, washed with 3L of water at 0-5°C, washed with 1L of ethanol at room temperature, and dried by blast at room temperature to obtain 928.36g of white crystalline solid with a yield of 75.21% and a purity of 99.6%.

Embodiment 3

[0031] Dissolve 3.2Kg of potassium hydroxide in 9.6L of water, add it into a 20L reaction kettle, cool down to 0-5°C, add 38g of potassium iodide, add 0.8kg of allantoin in batches, stir to dissolve, and control the temperature at 0-5°C It takes 9 hours to add 1.6kg bromine dropwise. After the dropwise addition, stir at 0-5°C for 1 hour, heat up to 20-25°C and react for 20 hours. HPLC detects that allantoin is <0.6%, cool down to 0-5°C, and add acetic acid dropwise to adjust pH to 5, filtered, washed with 3L of water at 0-5°C, washed with 1L of ethanol at room temperature, and air-dried at room temperature to obtain 712.07g of white crystalline solid with a yield of 72.1% and a purity of more than 99.8%.

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Abstract

The invention belongs to the technical field of chemical synthesis and particularly relates to a method for preparing potassium oxonate, comprising the following steps: dissolving potassium hydroxide in water, clarifying and then cooling to 0-5 DEG C, adding potassium iodide, adding allantoin in batch, stirring for dissolving, dropwise adding bromine at a controlled temperature of 0-5 DEG C for 7-11 h, stirring at 0-5 DEG C for 1 after dropwise adding, heating to 20-25 DEG C and reacting for 18-22 h, and detecting allantoin being <0.6% through HPLC (high performance liquid chromatography), cooling to 0-5 DEG C, dropwise adding acetic acid to adjust pH to 5, filtering, washing with water, washing with ethanol, and drying to obtain the potassium oxonate. The method has good reaction effect, high product yield and low cost, is simple to perform and is particularly applicable to industrial application.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing oteracil potassium. Background technique [0002] The chemical name of oteracil potassium is 1,2,3,4-tetrahydro-2,4-dicarbonyl-1,3,5-triazine-6-carboxylate potassium, and its structural formula is as follows: [0003] . [0004] One of the constituents of the new anticancer drug S-1, which can inhibit the toxic and negative effects of the anticancer drug tegafur. [0005] S-1 is a fluorouracil derivative oral anticancer agent, which includes tegafur (FT) and the following two types of modulators: gimeracil (CDHP) and oteracil (Oxo). The functions of its three components are as follows: FT is a prodrug of 5-Fu, which has excellent oral bioavailability and can be converted into 5-Fu in vivo. CDHP can inhibit the catabolism of 5-Fu released from FT under the action of dihydropyrimidine dehydrogenase. Note similar effects. Oxo can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/20
CPCC07D251/20
Inventor 马居良郭明刘怀振
Owner 山东川成医药有限公司
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