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A kind of sulfadiazine n-methylpyrrolidone solvent compound crystal and preparation method thereof

A technology of methylpyrrolidone and solvent compound, which is applied in the field of sulfadiazine N-methylpyrrolidone solvent compound and its preparation, can solve the problems of small crystal particle size, low solubility of sulfadiazine, poor crystal post-processing performance, etc., and achieve bulk density and fluidity improvement, and the effect of easy post-processing

Active Publication Date: 2017-05-17
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The solubility of sulfadiazine in water is very small, the crystal particle size is very small, and the post-treatment performance of the crystal is not good. The purpose of preparing the solvent compound is to develop a new crystal form of sulfadiazine, improve the solubility of sulfadiazine, and increase the particle size. Improved postprocessing performance of particles

Method used

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  • A kind of sulfadiazine n-methylpyrrolidone solvent compound crystal and preparation method thereof
  • A kind of sulfadiazine n-methylpyrrolidone solvent compound crystal and preparation method thereof
  • A kind of sulfadiazine n-methylpyrrolidone solvent compound crystal and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0035] Add 10g of anhydrous sulfadiazine to 15g of N-methylpyrrolidone solvent, dissolve rapidly, stir at 30°C for 30 minutes, it will be accompanied by nucleation and growth process, filter and dry the product to obtain sulfadiazine N-methylpyrrolidone solvate crystals, yield : 94.5%.

[0036] The XRD, TG spectrum and microscope picture of the test product and the attached figure 1 , attached figure 2 And attached image 3 Consistent, confirm that the obtained product is a new crystal form of sulfadiazine N-methylpyrrolidone.

Embodiment 2

[0038] Add 6g of sulfadiazine to 60g of N-methylpyrrolidone, dissolve after stirring at 25°C, continue to stir and crystallize slowly to generate sulfadiazine N-methylpyrrolidone solvate, filter and dry to obtain sulfadiazine N-methylpyrrolidone solvate product , Yield: 85.3%.

[0039] The XRD and TG patterns of the test product and the accompanying figure 1 And attached figure 2 unanimous. It is confirmed that the obtained product is a new crystal form of sulfadiazine N-methylpyrrolidone.

Embodiment 3

[0041] Add 5 g of sulfadiazine to 50 g of water with a water content of 30% and N-methylpyrrolidone mixed solvent, stir at 30°C for 2 hours, the clear solution slowly crystallizes, and produces a solvent compound, which is filtered and dried to obtain sulfadiazine N-methylpyrrolidone Pyrrolidone solvate crystals, yield: 92.3%.

[0042] The XRD and TG patterns of the test product and the accompanying figure 1 And attached figure 2 Consistent, confirm that the obtained product is a new crystal form of sulfadiazine N-methylpyrrolidone.

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Abstract

The invention provides a sulfadiazine N-methyl pyrrolidone solvate crystal and a preparation method thereof. Each molecule of the sulfadiazine N-methyl pyrrolidone solvate crystal contains one molecule of sulfadiazine and two molecules of N-methyl pyrrolidone; the X-ray powder diffraction pattern of the sulfadiazine N-methyl pyrrolidone solvate crystal shows characteristic peaks at diffraction angles 2theta, wherein 2theta can be 8.08+ / -0.1, 11.6+ / -0.1, 15.78+ / -0.1, 16.22+ / -0.1, 17.28+ / -0.1, 18.42+ / -0.1, 19.44+ / -0.1, 20.94+ / -0.1, 23.12+ / -0.1, 23.46+ / -0.1, 24.46+ / -0.1, 25.46+ / -0.1, 26.92+ / -0.1, 28.56+ / -0.1 and 31.12+ / -0.1. The preparation method is simple to operate. The yield is above 85% and the major granularity of the crystal is about 240 microns. After the sulfadiazine N-methyl pyrrolidone solvate is placed at a room temperature for more than three months, the XRD pattern has no change, and therefore, the crystal is excellent in stability.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering and medicine, and in particular relates to a sulfadiazine N-methylpyrrolidone solvent compound and a preparation method thereof. Background technique [0002] Sulfadiazine is an intermediate-acting sulfa drug. Molecular formula C 10 h 10 N 4 o 2 S, molecular weight 250.28, its chemical name is: N-2-pyrimidinyl-4-aminobenzenesulfonamide. The chemical structural formula is: [0003] [0004] Sulfa drugs were developed from azo dyes, and sulfadiazine was first synthesized in 1941. Sulfadiazine is currently a sulfonamide anti-infective drug commonly used clinically in my country. Sulfadiazine is effective against hemolytic streptococcus, staphylococcus, meningococcus, pneumococcus, gonorrhoeae, Escherichia coli, Shigella and other sensitive bacteria and Chlamydia trachomatis , Actinomycetes, Plasmodium, Star Nocardia and Toxoplasma gondii and other microorganisms have inhibitory ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/69C07D207/267
CPCC07B2200/13C07D207/267C07D239/69
Inventor 尹秋响吴送姑李康丽孙佳龚俊波侯宝红
Owner TIANJIN UNIV
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