Preparation method of nitrofurazone alpha crystal

A technology for nitrofurazone and crude nitrofurazone, which is applied in the field of drug crystallization, can solve the problems of non-concentrated particle size distribution, potential safety hazards, and small bulk density, and achieve the effects of increasing bulk density, good stability, and improving filtration properties

Active Publication Date: 2019-02-15
TIANJIN UNIV
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0006] After testing, the commercially available nitrofurazone is in the β crystal form. This crystal form has problems such as non-concentrated particle size distribution, easy aggregation, low bulk density, and potential safety hazards. Compared with the needle-shaped β crystal form and the flake γ crystal , bulky crystals have greater bulk density and better stability, so it is still necessary to study the nitrofurazone α crystal form that is easy to obtain, large bulk density, and good thermodynamic stability and a process that is convenient for industrial production, so as to ensure that the raw material drug and the stability of its preparations in preparation and storage, and improve the drug quality and clinical efficacy of nitrofurazone

Method used

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  • Preparation method of nitrofurazone alpha crystal
  • Preparation method of nitrofurazone alpha crystal
  • Preparation method of nitrofurazone alpha crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 15 g of dry nitrofurazone β crystal form to a mixed solution of 50 g N,N-dimethylformamide and 50 g methanol to form a suspension, keep the temperature of the suspension at 5°C while stirring, suspend and stir for 24 hours, and filter the suspension with suction , the product was dried to constant weight at 50°C under normal pressure to obtain nitrofurazone in α crystal form.

[0036] The X-ray powder diffraction of the crystal obtained in this embodiment is as follows: figure 1 As shown, it mainly has characteristic peaks at diffraction angles 2θ=8.782, 13.719, 15.443, 18.660, 20.581, 21.081, 22.998, 23.899, 24.200, 25.317, 26.638, 27.877, 30.238, 31.700, 35.182 °. The more comprehensive characteristic peaks are 衍射角2θ=8.782,13.719,15.443,17.622,18.660,20.581,21.081,22.998,23.899,24.200,25.317,26.638,27.877,30.238,31.700,33.202,34.001,35.182,36.880,37.321°,所以所得产品为α Crystalline nitrofurazone,

[0037] The characteristic peak temperature of the DSC diagram of the nit...

Embodiment 2

[0042] Add 16 g of dry nitrofurazone β crystal form to a mixed solution of 50 g formamide and 50 g acetonitrile to form a suspension, keep the temperature of the suspension at 20°C under stirring, suspend and stir for 11 hours, filter the suspension with suction, and put the product at 50°C , and dry to constant weight under normal pressure to obtain α-crystalline nitrofurazone.

[0043] The X-ray powder diffraction, DSC, infrared and Raman spectrum characterization data of the crystal obtained in this example are the same as those in Example 1, the UV purity is 98.62%, and the bulk density is 0.36g / cm 3 .

Embodiment 3

[0045] Add 2.8 g of dry nitrofurazone β crystal form to 10 g of dimethyl sulfoxide to form a suspension, keep the temperature of the suspension at 25°C under stirring, suspend and stir for 15 hours, filter the suspension with suction, and store the product at 80°C under normal pressure Drying to constant weight at 100°C yields α crystalline nitrofurazone.

[0046] The X-ray powder diffraction, DSC, infrared and Raman spectrum characterization data of the crystal obtained in this example are the same as those in Example 1, the UV purity is 98.56%, and the bulk density is 0.36g / cm 3 .

[0047] Ultrasound-assisted solvent-mediated crystallization:

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Abstract

The invention relates to a preparation method of nitrofurazone alpha crystal, and provides characterization data of DSC, infrared and Raman spectra of the nitrofurazone alpha crystal. The preparationmethod is solvent-mediated crystal transformation or ultrasonic assisted solvent-mediated crystal transformation. The predation method comprises the steps of adding crude nitrofurazone to an organic solvent to prepare a 0.12-0.40g solute/g solvent suspension, and then stirring the suspension at a constant temperature of 5-30 DEG C for 15-24 h; or performing ultrasonic treatment for 10-60 min whilestirring the suspension at a constant temperature of 5-30 DEG C, and then continuing to stir the suspension at a constant temperature of 5-30 DEG C for 5-18 h; and finally, filtering the suspension,and drying the crystal product at 50-80 DEG C to a constant weight. The nitrofurazone alpha crystal has a bulk density of 0.35-0.38g/cm3 and a purity of more than 98. 5%, and the method is simple andlow in energy consumption; and the crystal is easy to filter, good in thermodynamic stability, etc.

Description

technical field [0001] The invention belongs to the technical field of medicine crystallization, and in particular relates to a preparation method of nitrofurazone α crystal form. Background technique [0002] The Chinese chemical name of nitrofurazone is 5-nitro-2-furaldehyde semicarbazone, the English chemical name is 5-nitro-2-furaldehyde semi-carbazone, the CAS number is 59-87-0, and the molecular formula is C 6 h 6 N 4 o 4 , the molecular weight is 198.14. Its structural formula is shown in formula (I), [0003] [0004] Nitrofurazone is a synthetic antibiotic that has antibacterial effects on a variety of Gram-positive and negative bacteria. Usually, furfural is nitrated, esterified, and hydrolyzed to produce 5-nitrofurfural, and then condensed with hydrochloric acid amino group to obtain nitrofurazone. It was initially used to treat burns, skin infections, suppurative dermatitis, suppurative otitis media and other diseases because of its low tissue irritation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/76
CPCC07D307/76C07B2200/13
Inventor 郝红勋李欣黄欣李飞侯宝红尹秋响徐昭鲍颖谢闯王召
Owner TIANJIN UNIV
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