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A kind of preparation method of nitrofurazone γ crystal form

A technology for nitrofurazone and nitrofurazone crude products is applied in the field of crystalline preparation of nitroxide γ crystal form, and can solve the problems of inconcentrated particle size distribution, easy agglomeration, potential safety hazards and the like

Active Publication Date: 2022-03-15
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 coalescence, low bulk density, and potential safety hazards. Compared with needle-like and flaky crystals, blocky crystals have more Large bulk density and better stability

Method used

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  • A kind of preparation method of nitrofurazone γ crystal form
  • A kind of preparation method of nitrofurazone γ crystal form
  • A kind of preparation method of nitrofurazone γ crystal form

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Add 1.65 g of dry nitrofurazone α crystal form to 25 ml of N,N-dimethylformamide, control the temperature at 30°C, stir at 200 rpm for 30 min to dissolve, and filter through a 0.22 μm filter membrane to remove insoluble impurities. Add water at 0.3ml / min for 5 minutes until crystals emerge, then grow crystals for 30 minutes; add water at 0.3ml / min for 30 minutes, grow crystals for 30 minutes; add water at 0.6ml / min for 30 minutes, grow crystals for 30 minutes; add water at 1.8ml / min for 30 minutes, cool down to 5°C for 120 minutes, and keep the temperature constant Cultivate the crystal at 5°C for 30 minutes; suction and filter the feed solution, wash twice with 8ml of water each time, and dry the product at 50°C under normal pressure to constant weight to obtain nitrofurazone in the γ crystal form.

[0040] The X-ray powder diffraction of the crystal obtained in this embodiment is shown in the attached figure 1 所示,其在衍射角2θ=6.645,13.136,16.399,17.517,19.265,20.045,22.342...

Embodiment 2

[0045] Add 1.65 g of dry nitrofurazone α crystal form to 25 ml of N,N-dimethylformamide, control the temperature at 40°C, stir at 300 rpm for 20 min to dissolve, and filter through a 0.22 μm filter membrane to remove insoluble impurities. Add isopropanol at 0.5ml / min for 10min to produce crystals, then grow crystals for 30min; add isopropanol at 0.5ml / min for 30min, grow crystals for 30mins; Use isopropanol for 30 minutes, cool down to 5°C for 90 minutes, grow crystals at 5°C for 30 minutes at a constant temperature; pump and filter the feed solution, wash twice with 8ml of isopropanol each time, and dry the product at 60°C under normal pressure to constant weight to obtain Gamma crystalline form of nitrofurazone.

[0046] The X-ray powder diffraction of the crystal obtained in this example, the characterization data of infrared and Raman spectra are the same as those in Example 1, the UV purity is 98.85%, and the bulk density is 0.38g / cm 3 .

Embodiment 3

[0048] Add 1.80 g of dry nitrofurazone β crystal form to 20 ml of N,N-dimethylformamide, control the temperature at 50°C, stir at 400 rpm for 20 min to dissolve, and filter through a 0.22 μm filter membrane to remove insoluble impurities. Add n-propanol at 0.6ml / min for 15 minutes to produce crystals and grow crystals for 30 minutes; add n-propanol at 0.6ml / min for 15 minutes and grow crystals for 30 minutes; Propanol for 15 minutes, 100 minutes to cool down to 8°C, constant temperature at 8°C to grow crystals for 30 minutes; suction and filter the feed solution, wash twice with n-propanol 9ml / time, and dry the product at 70°C under normal pressure to constant weight to obtain γ Crystalline nitrofurazone.

[0049] The X-ray powder diffraction of the crystal obtained in this example, the characterization data of infrared and Raman spectra are the same as those in Example 1, the UV purity is 98.81%, and the bulk density is 0.40g / cm 3 .

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Abstract

The invention relates to a preparation method of nitrofurazone gamma crystal form. Add the crude nitrofurazone into a good solvent, control the temperature at 30-50°C, stir at 200rpm-500rpm until it dissolves, and prepare a solution of 0.066-0.24g / ml; filter the solution to remove insoluble impurities by suction filtration; use 0.3-0.6ml / Add the poor solvent dropwise in 1 minute until the crystals come out, and grow the crystal; then add the poor solvent dropwise in three stages from slow to fast; cool down to 5-10°C for 90-120 minutes, grow the crystal for 20-30 minutes; pump and filter the liquid, 7-9ml Wash twice with a poor solvent every time, and dry the crystal product to constant weight. The nitrofurazone γ crystal form provided by the present invention has a bulk density of 0.38 to 0.48 g / cm 3 , the purity is higher than 98.8%, has the advantages of simple process operation, short time consumption, low energy consumption, and is suitable for industrial production; the crystal is easy to filter, and the thermodynamic stability is good.

Description

technical field [0001] The invention belongs to the technical field of drug crystallization, and in particular relates to a crystallization preparation method of nitrofurazone gamma 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 t...

Claims

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Application Information

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Patent Type & Authority Patents(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