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Preparation method suitable for industrially producing oteracil potassium

A technology of oteracil potassium and potassium iodide, applied in the field of medicinal chemistry, can solve the problems of undisclosed final product purity and the like, and achieve the effects of reducing the use of organic solvents, saving costs, and having a simple refining method

Inactive Publication Date: 2013-11-13
深圳万乐药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The highest yield of this patented method is 70%. The final product is obtained by washing with water and acetone successively. The purity of the final product is not disclosed

Method used

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  • Preparation method suitable for industrially producing oteracil potassium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Dissolve 560g of potassium hydroxide in 2000ml of deionized water, cool to 0-5°C, add 8g of potassium iodide, cool to 0-5°C, add 158g of allantoin, slowly add 320g of bromine, and control the temperature at 1-5°C Reaction, after the dropwise addition, raise the temperature to 20°C and react for 30-40 hours until the reaction is complete, adjust the pH to 6±0.2 with glacial acetic acid while stirring, cool down to 0-5°C, stir and crystallize for one hour, filter with suction, add deionization to the solid 1000ml of water was stirred into a suspension, filtered with suction, and the filter cake was repeatedly washed with deionized water once, and dried to obtain 145g of crude product with a yield of 74%. The purity by HPLC was 98.5%, and there was one impurity with a content greater than 0.5%.

[0018] Add 2 L of deionized water to the crude product of oteracil potassium, slowly add 50% potassium hydroxide aqueous solution and stir until clarification, filter to remove ins...

Embodiment 2

[0020] Dissolve 510g of potassium hydroxide in 2000ml of deionized water, cool to 0-10°C, add 10g of potassium iodide, cool to 0-5°C, add 158g of allantoin, slowly add 400g of bromine, and control the temperature at 1-5°C Reaction, after the dropwise addition, raise the temperature to 20°C and react for 30-40 hours until the reaction is complete, adjust the pH to 6±0.2 with 15% hydrochloric acid under stirring, cool down to 0-5°C, stir and crystallize for one hour, filter with suction, and remove the solids 1000ml of deionized water was stirred into a suspension, suction filtered, and the filter cake was repeatedly washed with deionized water once, and dried to obtain 140g of crude product, with a yield of 71%, a purity of 98.7% by HPLC, and one impurity with a content greater than 0.5%;

[0021] Add 2 L of deionized water to the crude product of oteracil potassium, slowly add 50% potassium hydroxide aqueous solution and stir until clarification, filter to remove insoluble matt...

Embodiment 3

[0023] Dissolve 610g of potassium hydroxide in 2000ml of deionized water, cool to 5-10°C, add 13g of potassium iodide, cool to 0-5°C, add 158g of allantoin, slowly add 450g of bromine, and control the temperature at 1-5°C Reaction, after the dropwise addition, raise the temperature to 20°C and react for 30-40 hours until the reaction is complete, adjust the pH to 6±0.2 with 15% sulfuric acid under stirring, cool down to 0-5°C, stir and crystallize for 2 hours, filter with suction, and remove the solids 1000ml of deionized water was stirred into a suspension, suction filtered, and the filter cake was repeatedly washed with deionized water once, and dried to obtain 142g of crude product, with a yield of 73%;

[0024] Add 2 L of deionized water to the crude product of oteracil potassium, slowly add 50% potassium hydroxide aqueous solution and stir until clarification, filter to remove insoluble matter, add 15% sulfuric acid dropwise to the filtrate under stirring to adjust the pH ...

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Abstract

The invention provides a preparation method suitable for industrially producing oteracil potassium. The method provided by the invention has the advantages that: reaction steps are fewer, oxidants which generate gases polluting the environment are not used, a refining method is simple, the consumption of organic solvents which are harmful to the human body is decreased, the cost is saved, the total yield can reach more than 65%, and the method is suitable for the industrial production; the purity of a product reaches more than 99.8%, the impurity content of the single product is less than 0.1% and the purity and the impurity of the product both reach quality standards for the raw material medicine; and the obtained product is the oteracil potassium raw material medicine which is suitable for preparation of a medicinal preparation.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a preparation method of oteracil potassium, one of the components of the compound drug Siggio capsule. Background technique [0002] Oteracil Potassium is one of the three active drugs in the oral anti-cancer compound drug T-Gio Capsules, which is an oral anti-cancer agent of fluorouracil derivatives, mainly composed of Tegafur and two biochemical regulators Composed of gimester and oteracil potassium, tegafur has excellent oral bioavailability and can be converted into 5-fluorouracil in the body; gimester can inhibit the decomposition of 5-fluorouracil, making 5-fluorouracil in The plasma and tumor tissue maintain a stable blood concentration for a longer period of time, thereby enhancing anti-tumor activity; oteracil potassium can reduce the toxicity and adverse reactions of 5-fluorouracil in the gastrointestinal tract. The two biochemical modulators work together to enable ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/20
Inventor 王先登刘立力李瑞远张广明
Owner 深圳万乐药业有限公司
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