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Low-heat solid-phase synthesis method of heparin quaternary ammonium salt

A low-heat solid-phase synthesis method technology, which is applied in the low-heat solid-phase synthesis of heparin quaternary ammonium salts, and in the field of compound synthesis, to achieve the effect of less control parameters, simple operation, and easy control

Active Publication Date: 2011-05-04
石河子市郁茏生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Application of low-heat solid-phase synthesis to synthesize heparin quaternary ammonium salt has not been reported at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 12.0 g of heparin sodium and 36 mg of sodium chloride, mix and grind for 0.5 hour. Then add 14.4g of benzethonium chloride, 43.2mg of ferric oxide, under the protection of nitrogen (pressure 0.0005Mpa), grind at 90°C for 4 hours to obtain 26.0g of solid powder, yield 98.6%, HPLC, purity 98.5% .

Embodiment 2

[0029] Take 10.0 g of heparin sodium and 30 mg of sodium chloride, mix and grind for 0.5 hours. Add 12.0 g of benzethonium chloride, 36 mg of ferric oxide, and grind at 90° C. for 4 hours under the protection of nitrogen (pressure 0.0005 Mpa) to obtain 21.8 g of solid powder, with a yield of 98.8%, and a purity of 99.5% by HPLC.

Embodiment 3

[0031] Take 12.0 g of heparin sodium and 24 mg of sodium chloride, mix and grind for 0.5 hours. Then add 15.6g of benzethonium chloride, 31.2mg of ferric oxide, under the protection of nitrogen (pressure 0.0006Mpa), grind at 93°C for 4 hours to obtain 27.0g of solid powder, yield 97.6%, HPLC detection, purity 97.5% .

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Abstract

The invention discloses a low-heat solid-phase synthesis method of a heparin quaternary ammonium salt. In the method, the heparin quaternary ammonium salt is prepared by a low-heat solid-phase reaction by using heparin sodium and benzethonium chloride as raw materials, using sodium chloride and ferric oxide as mineralizers and using inert gas as a protective agent. The method has the advantages of thorough reaction, high yield, low energy consumption and less pollution, and is applicable to industrial production, thereby being a promising preparation method.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a low-heat solid-phase synthesis method of heparin quaternary ammonium salt, and belongs to the technical field of chemical synthesis. Background technique [0002] Enoxaparin is an anticoagulant and antithrombotic drug, which is a derivative of low molecular weight heparin sodium. Usually, enoxaparin is obtained from heparin through quaternization, esterification, and finally β-elimination in alkaline solution. [0003] The quaternization of heparin is a key step in the preparation of enoxaparin. Chinese patent (authorization number CN100582123C) discloses a method for quaternization of heparin, as follows: dissolve heparin sodium in 7 to 11 times of water at room temperature, adjust the pH to 7.0 to 9.0; Dissolve thormonium chloride in 3 to 7 times of water and stir evenly, add heparin sodium aqueous solution to benzethonium chloride aqueous solution, after full reaction, vacuum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/10
Inventor 姚成盛
Owner 石河子市郁茏生物科技有限公司
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