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Refining method for preparing gimeracil

A refining method, the technology of gimeracil, is applied in the field of drug synthesis, which can solve the problems of unrefined crude products, difficult to reach the pharmacopoeia standard, and low yield, and achieve strong operability, simple and feasible refining methods, and less side effects. Effect

Active Publication Date: 2015-02-04
SHANDONG NEWTIME PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The yield of this method is low, the crude product is not refined, and the purity is not mentioned
[0015] CN200680003210.X provides a preparation method of 5-chloro-2,4-dihydroxypyridine. After the reaction of 5-chloro-2,4-dihydroxypyridine is completed, the reaction solution is concentrated, and acid is added to the residue for separation or alkali is added Precipitate 5-chloro-2,4-dihydroxypyridinium salt separation, and then treat the final product with acid. The inventor found through high-performance liquid phase analysis that although the color of the product has improved by this method, the purity is difficult to reach the pharmacopoeia standard

Method used

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  • Refining method for preparing gimeracil
  • Refining method for preparing gimeracil
  • Refining method for preparing gimeracil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 30g of gimeracil into a beaker, add 140ml of water and stir, add 8% NaOH solution dropwise, adjust the pH to 9, heat in a water bath to 40°C to completely dissolve the solid, add 1.5g of activated carbon, stir for 15min, filter with suction, and repeat the decolorization once. The filtrate was adjusted to pH 3 with HCl with a concentration of 6% by mass, a white solid precipitated out, cooled, crystallized at -5°C for about 4 hours, filtered with suction, washed the filter cake twice with cold water, and the product was vacuum-dried to obtain 27.3 g of white or Off-white crystalline powder, yield 91%, purity 99.97%. (HPLC detection)

Embodiment 2

[0032] Add 30g of gimeracil into a beaker, add 150ml of water and stir, add dropwise 9% KOH solution, adjust the pH to 10, heat in a water bath to 50°C to completely dissolve the solid, add 1.5g of activated carbon, stir for 15min, filter with suction, repeat decolorization once, Adjust the pH of the filtrate to 4 with 10% acetic acid by mass percentage, a white solid precipitates out, cool to 0°C to crystallize for about 4 hours, filter with suction, wash the filter cake twice with cold water, and dry the product in vacuum to obtain 27.0 g of white or similar White crystalline powder, yield 90%, purity 99.96%. (HPLC detection)

Embodiment 3

[0034]Add 30g of gimeracil into a beaker, add 130ml of water and stir, add 7% NaOH solution dropwise, adjust the pH to 10, heat in a water bath to 50°C, and dissolve the solid completely, add 1.5g of activated carbon, stir for 15min, filter with suction, repeat decolorization once, The filtrate was adjusted to pH 3.5 with 6% sulfuric acid by mass percentage, white solids precipitated, cooled to -2°C to crystallize for about 4 hours, filtered with suction, washed the filter cake twice with cold water, and dried in vacuum to obtain 26.4g of white or off-white solids. White crystalline powder, yield 88%, purity 99.96%. (HPLC detection)

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Abstract

The invention belongs to the field of medicine synthesis, and especially relates to a refining method of a medicine compound gimeracil. According to the invention, a gimeracil crude product is added into water; alkali is added, and a pH is controlled at 9-11; the mixture is heated, until the crude product is completely dissolved; active carbon is added for discoloration; the pH is regulated to 3-4 by using an acid; crystallization is carried out at a temperature of -5 DEG C to 20 DEG C; and filtering and drying are carried out, such that gimeracil fine product is obtained. The yield is higher than 88%, and the purity is higher than 99.95%.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for refining the drug compound gimeracil. Background technique [0002] Gimeracil (Gimeracil), also known as Gimeracil, Gimeracil, chemical name: 5-chloro-2,4-dihydroxypyridine or 5-chloro-4-hydroxy-2(1H)-pyridone, chemical structure is as follows : [0003] [0004] Gimeracil is an ingredient of S-1 Capsules. The drug was first developed by Dapeng Pharmaceutical Co., Ltd. in Japan. It consists of three ingredients: Tegafur, Gimeracil and Potassium Oxonate. It is approved in Japan for gastric cancer and head and neck cancer. cancer treatment. Gimeracil is added to the S-1 capsule as a biochemical regulator. The role of Gimeracil is to improve the anticancer efficacy of FT. When FT is taken orally into the body, it will first be converted into 5-FU under the catalysis of liver P450 activating enzyme, and then removed. About 10% enters the intestinal tract and is phosph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/69
Inventor 赵志全
Owner SHANDONG NEWTIME PHARMA