Method for preparing doxofylline

A technology of doxofylline and theophylline, applied in the field of preparation of doxofylline, can solve problems such as product pollution, and achieve the effect of digesting organic solvent residues

Inactive Publication Date: 2013-02-20
KAIFENG MINGREN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a method of using purified water as a solvent for the deficiencies in the prior art of doxofylline synthesis (that is, the defect that organic solvents are used in the existing synthesis method...

Method used

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  • Method for preparing doxofylline
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  • Method for preparing doxofylline

Examples

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Embodiment 1

[0033] In the preparation method of doxofylline of the present invention, the detailed steps of the preparation method are as follows:

[0034] a. Take anhydrous theophylline and bromoacetaldehyde ethylene glycol as basic raw materials, use purified water as solvent, and anhydrous sodium carbonate as acid binding agent;

[0035] The mass ratio of the added amount between the anhydrous theophylline and bromoacetaldehyde ethylene glycol is 1:1.02, and the mass ratio of the added amount between the anhydrous theophylline and purified water is 1:10, The mass ratio between anhydrous theophylline and anhydrous sodium carbonate is 1:0.97;

[0036] b. Prepare various raw materials in the ratio between the raw materials described in step a. First, add 10.0 g of anhydrous theophylline, 9.7 g of anhydrous sodium carbonate and 100 ml of solvent purified water into the reaction vessel, and then heat to 100 ℃, keep stirring and refluxing during heating to completely dissolve the anhydrous theophy...

Embodiment 2

[0041] In the preparation method of doxofylline of the present invention, the detailed steps of the preparation method are as follows:

[0042] a. Take anhydrous theophylline and bromoacetaldehyde ethylene glycol as basic raw materials, use purified water as solvent, and anhydrous sodium carbonate as acid binding agent;

[0043] The mass ratio of the added amount between the anhydrous theophylline and bromoacetaldehyde glycol acetal is 1:1.2, and the mass ratio of the added amount between the anhydrous theophylline and purified water is 1:9, The mass ratio between the anhydrous theophylline and anhydrous sodium carbonate is 1:0.6;

[0044] b. Prepare various raw materials in the ratio between the raw materials described in step a. First, add 10.0 g of anhydrous theophylline, 6.0 g of anhydrous sodium carbonate and 90 ml of solvent purified water into the reaction vessel, and then heat to 110 ℃, keep stirring and refluxing during heating to completely dissolve the anhydrous theophyll...

Embodiment 3

[0049] In the preparation method of doxofylline of the present invention, the detailed steps of the preparation method are as follows:

[0050] a. Take anhydrous theophylline and bromoacetaldehyde ethylene glycol as basic raw materials, use purified water as solvent, and anhydrous sodium carbonate as acid binding agent;

[0051] The mass ratio of the added amount between the anhydrous theophylline and bromoacetaldehyde glycol acetal is 1:1.0, and the mass ratio of the added amount between the anhydrous theophylline and purified water is 1:11, The mass ratio between anhydrous theophylline and anhydrous sodium carbonate is 1:0.85;

[0052] b. Prepare various raw materials in the ratio between the raw materials described in step a. First, add 10.0 g of anhydrous theophylline, 8.5 g of anhydrous sodium carbonate and 110 ml of solvent purified water into the reaction vessel, and then heat to 105 ℃, keep stirring and refluxing during heating to completely dissolve the anhydrous theophylli...

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Abstract

The invention discloses a method for preparing doxofylline. The preparation method comprises that anhydrous theophylline and bromoacetaldehyde ethylene acetal serve as basic materials, purified water serves as a solvent, and anhydrous sodium carbonate serves as a deacid reagent; the materials of the anhydrous theophylline, the anhydrous sodium carbonate and the solvent of the purified water are added in a reaction vessel to be stirred and heated, so that the anhydrous theophylline is dissolved completely; adding dropwise the bromoacetaldehyde ethylene acetal to perform reflux reaction, cooling crystallization and suction filtration are performed to obtain coarse product doxofylline; and the solvent of the purified water is added to dissolve the coarse product completely, activated carbon is added for decoloration, and cooling crystallization, suction filtration and drying are performed after decoloration to obtain the finished product doxofylline. According to the method for preparing doxofylline, the purified water is used as the solvent instead of organic solvents, so that the problem of residual organic solvent in a prior doxofylline preparation process is solved, and the doxofylline is conducive to being taken by patients.

Description

technical field [0001] The invention relates to a preparation method of xanthine compounds, in particular to a preparation method of doxofylline. Background technique [0002] Doxofylline (Doxofylline) is a new phenyline drug, a derivative of xanthine, and its chemical name is 1,3-dimethyl-7-(1,3-dioxol-2-yl) Methyl-3,7-dihydro-1H-purine-2,6-dione. Doxofylline is a bronchodilator that acts directly on the bronchi to relax bronchial smooth muscle. Doxofylline is a new generation of phosphodiesterase inhibitor antiasthma and antitussive drug, which is a derivative of methylxanthine, developed by Italian Rebberts Company, and was produced and marketed abroad in 1988. It is clinically used for the treatment of bronchial asthma, asthmatic chronic bronchitis and other dyspnea caused by bronchospasm. [0003] Doxofylline is a new type of phosphodiesterase inhibitor class of anti-asthma and antitussive drugs. Phosphodiesterase inhibitor drugs mainly refer to theophylline series ...

Claims

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Application Information

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IPC IPC(8): C07D473/08
Inventor 王国强王斐张宝国张宏波刘向前马俊萍
Owner KAIFENG MINGREN PHARMA
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