Benzbromarone crystal form A and preparation method thereof

A technology of benzbromarone crystal form and benzbromarone, which is applied in the field of chemical pharmaceuticals, can solve the problems of poor industrial applicability of crystallization purification methods, poor drug form stability, and inestimable market potential, achieving low cost and good crystal form stability , the effect of mild conditions

Active Publication Date: 2015-01-07
NORTHEAST PHARMA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since Benzbromarone entered my country in 2000, it has occupied the No. 1 position of anti-gout drugs in hospitals. Moreover, the market share of Benzbromarone is still on the rise, and its market potential is hard to estimate
[0004] Through the search of Chinese patents, it is found that most of the existing patents are the protection of the preparation method of benzbromarone synthesis or different dosage forms and uses. After searching the literature and domestic and foreign patents, no reports about the crystal form of benzbromarone have been found, and the existing drug forms Poor stability, high content of related substances, poor industrial applicability of crystallization purification method

Method used

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  • Benzbromarone crystal form A and preparation method thereof
  • Benzbromarone crystal form A and preparation method thereof
  • Benzbromarone crystal form A and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of benzbromarone crystal form A:

[0019] Take 27.5g of benzbromarone raw material and completely dissolve it in 90ml of acetone solvent under the condition of reflux at 56°C. After dissolving, the temperature is rapidly lowered, and solids are gradually precipitated, left to stand at 5°C for crystallization for 10 hours, filtered, and rinsed with a small amount of cold acetone , the benzbromarone crystal form A can be obtained.

[0020] The powder X-ray diffraction pattern of gained benzbromarone crystal form A is as attached figure 2 shown.

[0021] The infrared absorption spectrum figure of gained benzbromarone crystal form A is as attached image 3 shown.

[0022] The differential scanning calorimetry differential thermal analysis spectrum of gained benzbromarone crystal form A is as attached Figure 4 shown.

[0023] The detection method and result of differential scanning calorimetry differential thermal analysis spectrum are as follows:

[0024]...

Embodiment 2

[0032] Take 27.5g of benzbromarone raw material and completely dissolve it in 82ml of acetone solvent at 50°C. After dissolving, the temperature is rapidly lowered, and solids are gradually precipitated. Stand at 0°C for crystallization for 2 hours, filter, and rinse with a small amount of cold acetone. The crystal form A of benzbromarone can be obtained.

Embodiment 3

[0034] Take 27.5g of benzbromarone raw material and completely dissolve it in 138ml of acetone solvent at 40°C. After dissolving, the temperature is rapidly lowered, and solids are gradually precipitated. Stand at 20°C for crystallization for 15 hours, filter, and rinse with a small amount of cold acetone. The crystal form A of benzbromarone can be obtained.

[0035] The content of related substances of the benzbromarone crystal form A obtained by the preparation method of the present invention is far less than the standard of European Pharmacopoeia Version 7.0 (page 1465-1466), and the contents of related substances are shown in Table 1.

[0036] Table 1 Comparison of related substances of benzbromarone raw materials and crystal form A samples with European Pharmacopoeia standards

[0037]

[0038] The solid state of benzbromarone crystal form A obtained by this preparation method is respectively subjected to 10 days, 20 days, and 30 days under the conditions of 92.5% humi...

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Abstract

The invention relates to a benzbromarone crystal form A applicable to the field of chemical pharmacy and a preparation method thereof. In an X-ray powder diffraction pattern represented by a 2theta angle, the error range of the 2theta angle is +/- 0.2. The benzbromarone crystal form A has the basic X-ray powder diffraction pattern. In the differential scanning calorimetry pattern, when the heating speed is 10 DEG C per minute, the benzbromarone crystal form A has a maximal endothermic peak, and the melting point value of the benzbromarone crystal form A is 152.23 DEG C. The method comprises the following steps: under the condition of 25 DEG C, taking 1.0g of benzbromarone crystal form A, and adding 10ml of trichloromethane, wherein the solid is completely dissolved, and the solution is clear; taking 1.25g of benzbromarone crystal form A, and adding 25ml of N,N-dimethylformamide, wherein the solid is slightly insoluble, and the solution is not clear; and crystallizing from a single solvent acetone to obtain the benzbromarone crystal form A. The crystal form has the advantages of high stability, simple preparation method, low cost, simple after-treatment, high product purity and fewer related substances.

Description

technical field [0001] The invention relates to a benzbromarone crystal form A in the field of chemical pharmacy and a preparation method thereof. Background technique [0002] Benzbromarone, also known as benzobromone, tongfenglixian, tongfengning, etc. This product is a derivative of benzofuran, which can inhibit the reabsorption of uric acid by renal tubules and thus reduce the concentration of uric acid in blood. It is easily absorbed orally, and its metabolites are effective. The uric acid in the blood 24 hours after taking the medicine is 66.5% of that before taking the medicine. For the treatment of gout. [0003] Benzbromarone was launched in Germany in 1971, licensed under the trade name of Urinorm in August 1978, and started selling tablets in April 1979. Since Benzbromarone entered my country in 2000, it has occupied the No. 1 position of anti-gout drugs in hospitals. Moreover, the market share of Benzbromarone is still on the rise, and its market potential is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/80
CPCC07B2200/13C07D307/80
Inventor 祝春艳胡铁军李想何艳艳刘素娜阎欢陈静白跃飞
Owner NORTHEAST PHARMA GRP
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