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A kind of preparation method of nitrofurazone α crystal form
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A technology for nitrofurazone and crude nitrofurazone, which is applied in the field of drug crystallization and can solve problems such as potential safety hazards, easy coalescence, and small bulk density
Active Publication Date: 2022-03-29
TIANJIN UNIV
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[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 materialdrug and the stability of its preparations in preparation and storage, and improve the drug quality and clinical efficacy of nitrofurazone
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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-raypowderdiffraction 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-raypowderdiffraction, 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-raypowder 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 .
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Abstract
The invention relates to a preparation method of nitrofurazone α crystal form, and simultaneously provides DSC, infrared and Raman spectrum characterization data of nitrofurazone α crystal form. The preparation method is solvent-mediated crystallization or ultrasonic-assisted solvent-mediated crystallization. Add the crude nitrofurazone into an organic solvent to form a suspension of 0.12-0.40g solute / g solvent, then suspend and stir at a constant temperature of 5-30°C for 15-24h; After ~60 minutes, continue to suspend and stir at a constant temperature of 5~30°C for 5~18h; finally filter the suspension with suction, and dry the crystal product at 50~80°C until it reaches a constant weight. The nitrofurazone α crystal form provided by the present invention has a bulk density of 0.35-0.38 g / cm 3 Among them, the purity is higher than 98.5%, and it has the advantages of simple process operation, low energy consumption, easy filtration of crystals, and good thermodynamic stability.
Description
technical field [0001] The invention belongs to the technical field of medicinecrystallization, 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-furaldehydesemicarbazone, 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...
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