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Amorphous crystal of tylonolide, and preparation method thereof

A new, amorphous technology of Tedirosan, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., to achieve simple process steps, high purity, and reduce the effect of organic solvent residues

Inactive Publication Date: 2014-02-05
QILU ANIMAL HEALTH PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the new amorphous crystal of Tediro has not been reported

Method used

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  • Amorphous crystal of tylonolide, and preparation method thereof
  • Amorphous crystal of tylonolide, and preparation method thereof
  • Amorphous crystal of tylonolide, and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0034] Preparation of New Amorphous Crystal of Tediro

[0035] Add 50 g of crystalline Tedirosin to 1000 ml of 0.1 mol / L phosphoric acid solution, stir to dissolve, slowly add 0.1 mol / L sodium hydroxide solution dropwise to adjust the pH of the reaction system to 10.0, keep the temperature at 20°C, and stir for 1 hour. Suction filtration and vacuum drying at 50°C for 12 hours gave 48.0 g of Tedirosin amorphous crystals with a purity of 99.50% and a water content of 0.84% ​​by HPLC.

Embodiment 2

[0037] Preparation of New Amorphous Crystal of Tediro

[0038] Add 50 g of crystalline Tedirosin to 500 ml of 0.5 mol / L sulfuric acid solution, stir to dissolve, slowly add 0.5 mol / L potassium hydroxide solution dropwise to adjust the pH value of the reaction system to 8.0, keep the temperature at 25 ° C, stir for 1 h, pump Filtrated, dried in vacuo at 65°C for 12 hours to obtain 49.1 g of Tedirosin amorphous crystals with a purity of 99.20% and a water content of 0.73% by HPLC.

Embodiment 3

[0040] Preparation of New Amorphous Crystal of Tediro

[0041] Add 50 g of crystalline Tedirosin to 250 ml of 1.0 mol / L hydrochloric acid, stir to dissolve, slowly add 1.0 mol / L sodium carbonate solution dropwise to adjust the pH of the reaction system to 9.0, keep the temperature at 30°C, stir for 1 hour, and filter with suction. Vacuum drying at 80°C for 12 hours yielded 49.5 g of amorphous crystals of Tedirosin with a purity of 99.11% and a water content of 0.85% by HPLC.

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Abstract

The invention relates to an amorphous crystal of tylonolide, and a preparation method thereof. The TG-DSC spectrum of the amorphous crystal of tylonolide has an endothermic peak between 185DEG C and 210DEG C, and has an exothermic peak between 140DEG C and 175DEG C; and the XRPD atlas of the amorphous crystal of tylonolide contains no identifiable diffraction peak shapes. The invention also provides the preparation method of the amorphous crystal of tylonolide. The tylonolide having a new crystal form has the advantages of good dissolvability, good stability, good bioavailability, simple preparation, no need of a special apparatus, low production cost, and suitableness for the industrialized production.

Description

technical field [0001] The invention relates to a new amorphous crystal of tediroate and a preparation method thereof, belonging to the technical field of preparation of veterinary antibiotics. Background technique [0002] Tedirosin, molecular formula: C 41 h 71 N 3 o 8 Molecular weight: 734.02, chemical name: 20-deoxy-23-deoxy-5-oxo-[3,6-dideoxy-3-(dimethylamino)-β-D-glucopyranosyl]-20,23- Dipiperidinyl Tylenolide, whose structural formula (Formula I), is a broad-spectrum macrolide antibiotic developed by Intervet-Schering-Plough. In March 2011, the European Union (CVMP) approved the marketing of its injection. In veterinary medicine, it is mainly used for the treatment of bovine respiratory tract infection caused by Mannheimia haemolytica, Pasteurella multocida and Haemophilus somnus and by Actinobacillus pleuropneumoniae, Pasteurella multocida, bronchial sepsis wave Respiratory tract infection of pigs caused by Haemophilus parasuis and Haemophilus parasuis. [000...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00
Inventor 方明锋刘全才李永东孔梅吴连勇
Owner QILU ANIMAL HEALTH PROD
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