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Sulfasalazine crystal form and preparation method thereof

A technology for sulfasalazine crystal and crystal form, which is applied to the crystal form of sulfasalazine and the field of preparation thereof, can solve the problems of not giving up research and the like, and achieve the effects of large crystal particle size and high dry rate

Inactive Publication Date: 2018-07-10
JIANGSU RUIKE MEDICAL SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Many literatures have studied the crystal form of sulfasalazine and metal complexes. Although the general trend is to move closer to the complex crystal form, the researchers of the present invention have not given up on sulfasalazine single crystal further research on

Method used

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  • Sulfasalazine crystal form and preparation method thereof
  • Sulfasalazine crystal form and preparation method thereof
  • Sulfasalazine crystal form and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 31g of crude sulfasalazine (wet product) and 50ml of DMF to the reaction flask, stir and heat up to 95-100°C, dissolve it, add 90ml of glacial acetic acid dropwise, keep warm after dropping, and start to cool down to 25- 30°C; after cooling down, heat preservation; after heat preservation, suction filtration and rinsing with 15ml of glacial acetic acid to obtain a wet product; vacuum drying to obtain 11.2g of product, yield 74.7%, HPLC purity 98.1%, after refining, HPLC purity 99.9 %. Powder X-ray Diffraction Pattern See figure 1 , the particle size detection result is D 10 : 6.4 μm, D 50 : 23.8 μm, D 90 : 46.9 μm. Its infrared spectrum is shown in image 3 .

Embodiment 2

[0042] Add 31g of crude sulfasalazine (wet product) and 50ml of DMF to the reaction flask, stir and heat up to 95-100°C, dissolve it, add 90ml of glacial acetic acid dropwise, keep warm after dropping, and start to cool down to 25- 30°C; after cooling down, heat preservation; after heat preservation, suction filtration and rinsing with 15ml of glacial acetic acid to obtain a wet product; vacuum drying to obtain 11.3g of product, yield 75.3%, HPLC purity 98.0%, after refining, HPLC purity 99.9 %. Powder X-ray Diffraction Pattern See figure 2 , the particle size detection result is D 10 : 5.8 μm, D 50 : 28.7 μm, D 90 : 61.0 μm. Its infrared spectrum is shown in Figure 4 .

Embodiment 3

[0044] Add 31g of crude sulfasalazine (wet product) and 50ml of DMSO to the reaction flask, stir and heat up to 95-100°C, dissolve, add 90ml of propionic acid dropwise, after the dropwise addition, add the new crystal form prepared in Example 1 Seed crystals, heat preservation; after heat preservation, start to cool down to 25-30°C; after cooling down, keep heat; after heat preservation, filter with suction, and rinse with 15ml propionic acid to obtain a wet product; vacuum dry to obtain 10.3g of the product, with a yield of 68% , HPLC purity 98.12%. It was determined by powder X-ray diffraction pattern detection that it was the same as Example 1, both of which were new crystal forms of sulfasalazine.

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Abstract

The invention belongs to the field of chemical pharmaceuticals, and relates to a sulfasalazine crystal form and a preparation method thereof. The method comprises the steps that two batches of the sulfasalazine crystal form are taken, and after powder X-ray diffraction is conducted, the main peaks are 2theta=26.516 and 2theta=26.425 respectively. Specifically, for the batch with the main peak of 2theta=26.516, characteristic peaks exist at the positions where the reflection angles 2theta of a powder X-ray diffraction pattern of the crystal form are 9.797+ / -0.2, 16.264+ / -0.2, 20.381+ / -0.2, 21.082+ / -0.2, 24.429+ / -0.2, 24.735+ / -0.2, 25.515+ / -0.2 and 26.516+ / -0.2, and for the batch with the main peak of 2theta=26.425, characteristic peaks exist at the positions where the reflection angles 2theta of the powder X-ray diffraction pattern of the crystal form are 9.761+ / -0.2, 16.257+ / -0.2, 20.353+ / -0.2, 21.045+ / -0.2, 24.407+ / -0.2, 24.741+ / -0.2, 25.468+ / -0.2 and 26.425+ / -0.2.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a crystal form of sulfasalazine and a preparation method thereof. Background technique [0002] 5-[p-(2-pyridinesulfamoyl)benzene]azosalicylic acid, the common name is sulfasalazine, and the CAS number is 599-79-1. It was launched in the United States in 1950 and in China in 1999. It is a very old product, but the market demand is still great. The main dosage forms are tablets and capsules, which are used to treat inflammatory bowel disease and ulcerative colitis. [0003] The literature Acta Crystallographica, Section C: Crystal Structure Communications (2001), C57 (4), 435-436 specifically described the reasons for the existence of polymorphs of sulfasalazine, and deduced that if the X-ray diffraction method is used to determine sulfasalazine Pyridine crystal form, the main peak should be at 2θ=26.53 Location. Since this is only an inference, and ...

Claims

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Application Information

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IPC IPC(8): C07D213/76
CPCC07D213/76C07B2200/13
Inventor 徐巧巧刘声民张军王长发叶美其高照波
Owner JIANGSU RUIKE MEDICAL SCI & TECH CO LTD
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