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Refining method of valnemulin hydrochloride

A technology of vonimulin hydrochloride and a refining method, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of sulfides, etc., can solve the problems of high equipment cost, difficulty in solvent recovery, physical injury of operators, etc. The use of expensive equipment, obvious purification effect, and the effect of reducing production costs

Active Publication Date: 2014-01-01
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the strong acidity of the aqueous solution of warnimulin hydrochloride, it is highly corrosive to the spray drying tower, and the equipment cost is high; if freeze drying is used, the equipment cost is high, and the product cannot be purified and refined
Chinese patent CN102001980 discloses a discharge method of warnemulin hydrochloride, that is, the crystallization method is used to obtain the solid of warnemulin hydrochloride, which can reduce the use and operation of equipment and purify the product, but the method The method introduces a variety of solvents in the preparation process, which increases the solvent residue in the product, and at the same time increases the difficulty of solvent recovery, pollutes the environment, and has certain harm to the operator's body
Chinese patent CN101456833 discloses a method for purifying warnemulin hydrochloride. After the method adopts warnemulin and ketone to react, deprotection, so as to achieve the purpose of purifying warnemulin hydrochloride, but the method steps are relatively cumbersome and increase The yield is greatly reduced after the reaction step

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 500ml of the methyl tert-butyl ether solution of vonimoulin base with a mass-volume concentration of 5%, add 0.5 times the volume of the above solution (ie 250ml purified water), heat to 40℃, stir for 0.5h, Set the layers, take the upper organic phase, and discard the lower aqueous phase. Add 600 ml of ethanol solution with a mass volume concentration of 10% to the organic phase, stir at room temperature for 0.5 h, stand still for layering, take the upper organic phase, and discard the lower aqueous phase. Pour dry hydrogen chloride gas into the organic layer obtained above, stir slowly at room temperature for 2 hours, and precipitate a large amount of crystals. At a rate of 5°C per hour, slowly lower the temperature to 0°C to complete the crystallization. The precipitated product is filtered. After drying, the solid product of Vonimulin Hydrochloride is obtained. Product yield: 99%. Purity: 99.8%. Moisture: 1.2%. Residual solvent: 6.2?? g / ml. Total impurities:...

Embodiment 2

[0023] Take 500ml of the methyl tert-butyl ether solution of Vonimulin base with a mass-volume concentration of 6%, add 300ml of purified water, heat to 40℃, stir for 1h, stand still for layering, take the upper organic phase, and discard the lower layer water box. Add 500 ml of ethanol solution with a mass volume concentration of 13% to the organic layer, stir at room temperature for 0.5 h, stand still for layering, take the upper organic phase, and discard the lower aqueous phase. Pour dry hydrogen chloride gas into the organic layer obtained above, stir slowly at room temperature for 3 hours, and precipitate a large amount of crystals. At a rate of 4°C per hour, slowly lower the temperature to 0°C to complete the crystallization. Filter the precipitated product. After drying, the solid product of Vonimulin Hydrochloride is obtained. Product yield: 98%. Purity: 99.2%. Moisture: 1.5%. Residual solvent: 5.6?? g / ml. Total impurities: less than 0.8%.

Embodiment 3

[0025] Take 500ml of the methyl tert-butyl ether solution of Vonimulin base with a mass-volume concentration of 7%, add 300ml of purified water, heat to 50℃, stir for 1h, stand still for layering, take the upper organic phase, and discard the lower layer water box. Add 700 ml of an ethanol solution with a mass volume concentration of 15% to the organic layer, stir at room temperature for 1 h, stand still for layering, take the upper organic phase, and discard the lower aqueous phase. Pour dry hydrogen chloride gas into the organic layer obtained above, stir slowly at room temperature for 3 hours, and precipitate a large amount of crystals. At a rate of 5°C per hour, slowly lower the temperature to 0°C and complete the crystallization. The precipitated product is filtered. After drying, the solid product of Vonimulin Hydrochloride is obtained. Product yield: 98.8%. Purity: 98.9%. Moisture: 1.8%. Residual solvent: 8.9?? g / ml. Total impurities: less than 1%.

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Abstract

The invention relates to a refining method of valnemulin hydrochloride. The refining method comprises the following steps: adding purified water or distilled water into an ether solution of valnemulin alkali; mixing; heating the solution until the temperature of the solution reaches 40-50 DEG C; stirring for 0.5-1h; standing for layering; taking the supernatant; adding an ethanol solution into the supernatant; stirring for 0.5-1h; standing for layering; taking the supernatant organic liquid; leading dry hydrogen chloride gas into the supernatant organic liquid; slowly stirring for 2-3h at the room temperature; separating out a large number of crystals; slowly reducing the temperature of the solution to 0 DEG C; filtering after completely crystallizing; drying the crystals. According to the refining method, the characteristics that the valnemulin alkali can be dissolved in the ether solution and the valnemulin hydrochloride cannot be dissolved in the ether solution are utilized, the valnemulin is become into a salt and then separated out through crystallization; the water and the ethanol solution are used for washing the valnemulin alkali so as to remove inorganic salt impurities and organic impurities from the valnemulin alkali, thus achieving a purifying purpose. The refining method has the characteristics of simple process, easy implementation in production, low cost, no pollution, relatively-high yield and high product purity.

Description

Technical field [0001] The invention relates to a preparation method of vornemulin hydrochloride, in particular to a method for refining vornemulin hydrochloride from vornemulin base. Background technique [0002] Valnemulin is a derivative of Pleuromutilin, which belongs to the semi-synthetic diterpenoid antibiotic, which is the same antibiotic as tiamulin. Vonimulin is mainly used for the prevention and treatment of mycoplasma and gram-positive infections in pigs, cattle, sheep and poultry. It has a broad antibacterial spectrum, strong resistance to bacteria, excellent pharmacokinetic characteristics, and residual The medicine in the body is low, safe and non-toxic. Vonimulin is an animal-specific antibiotic certified by the EU CEP and has a good market prospect. At present, it is mainly used in the form of amorphous hydrochloride in the market. [0003] At present, the preparation of vornemulin hydrochloride mainly involves mixing an aqueous hydrochloric acid solution with an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/20C07C319/28
Inventor 王义周丽娜王彬
Owner 宁夏泰瑞制药股份有限公司
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