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Oteracil potassium preparation method

A technology of oteracil potassium and potassium iodide, which is applied in the field of drug synthesis, can solve the problems of high bromine toxicity, potential safety hazards, and large pollution, and achieve the effects of high product yield, stable quality, and simple raw materials

Inactive Publication Date: 2015-05-13
BEIJING MEDISAN TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material allantoin used has been industrially produced on a large scale in China, and the price is cheap. However, the oxidant bromine used in this method is more toxic and pollutes the environment. The strong alkali reaction in the reaction heat is obvious, which has brought safety hazards to industrial production.

Method used

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Examples

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Embodiment 1

[0032] The preparation of embodiment 1 oteracil potassium

[0033] At room temperature, dissolve 336g potassium hydroxide (6mol) in 1200ml purified water, add 4.8g potassium iodide (0.03mol), add 95g allantoin (0.6mol), stir for 30min, add potassium persulfate 33g (0.12mol) in batches , stirred at room temperature for 24 hours until the reaction of the raw materials was complete, filtered off the insoluble matter, adjusted the pH of the filtrate to 6 with sulfuric acid, precipitated a solid, and dried to obtain 312 g of the product, with a purity of 99.8% and a maximum of 0.05%.

[0034] The solid-state nuclear magnetic resonance and HPLC analysis of gained product:

[0035] Test method: solid-state nuclear magnetic resonance is tested with a 500MHz nuclear magnetic resonance spectrometer. Data acquisition conditions: 13C CP / MAS NMR, 8kHz rotational speed, adamantane calibration (29.5ppm), contact time 2ms, pulse delay 8s. Timing 1h.

[0036] The solid-state NMR spectrum of...

Embodiment 2

[0037] The preparation of embodiment 2 oteracil potassium

[0038] At room temperature, dissolve 770g potassium carbonate (6mol) in 1200ml purified water, add 4.8g potassium iodide (0.03mol), add 95g allantoin (0.6mol), stir for 30min, add potassium persulfate 33g (0.12mol) in batches, Stir at 40°C until the reaction of the raw materials is complete, filter out the insoluble matter, add glacial acetic acid to the filtrate to adjust the pH to 6, precipitate a solid, and dry to obtain 338g of the product with a purity of 99.8% and a maximum of 0.02%.

Embodiment 3

[0039] The preparation of embodiment 3 oteracil potassium

[0040] At room temperature, dissolve 336g potassium hydroxide (6mol) in 1200ml purified water, add 95g allantoin (0.6mol), add 4.8g potassium iodide (0.03mol), stir for 30min, add potassium persulfate 33g (0.12mol) in batches , Stir at 30°C until the reaction of the raw materials is complete, filter out the insoluble matter, adjust the pH of the filtrate to 6±0.5 with hydrochloric acid, precipitate a solid, and dry to obtain 306g of the product with a purity of 99.8% and a maximum of 0.042%.

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Abstract

The invention discloses an oteracil potassium preparation method whcih comprises the following steps: allantoin is dissolved in the aqueous solution of potassium hydroxide or potassium carbonate, potassium iodide is used as a catalyst, potassium persulfate is used as an oxidant to synthesize oteracil potassium. Reaction steps of the method are short, the environmentally-friendly and cheap oxidant is used, use of toxic and harmful oxidant can be avoided, and the method has the advantages of simple operation, mild reaction condition, high yield, pure product, no any environmental pollution and the like, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of medicine synthesis, in particular to a preparation method of the medicine compound oteracil potassium. Background technique [0002] Oteracil potassium, also known as potassium oxonate, chemical name: potassium 1,4,5,6-tetrahydro-4,6-dioxo-1,3,5-triazine-2-carboxylate, chemical The structural formula is as follows: [0003] [0004] Oteracil potassium is one of the three components (tegafur, gimeracil, and oteracil potassium) of the antigastric cancer drug cefecone (S-1). As a commonly used anti-gastric cancer drug in clinical practice, Tegafur has limitations such as incomplete oral absorption, short half-life (5-20 min), rapid metabolism, and adverse reactions such as diarrhea. Tegafur is a prodrug of 5-fluorouracil, which has a good oral absorption effect and is gradually converted into 5-fluorouracil in the liver. Gimostel inhibits the degradation of 5-fluorouracil by inhibiting dihydropyrimidine dehydrog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/20
CPCC07D251/20
Inventor 王明新刘津爱杨帆廖凯俊朱岩周梦君
Owner BEIJING MEDISAN TECH
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