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Preparation method of valnemulin and hydrochloride thereof

A technology of warnimulin and hydrochloride, which is applied in the field of preparation of antibiotics, can solve the problems that the purity cannot be used as medicine, there is no patent, and the requirements for stirring and refrigeration are high, and the effect of mild conditions, easy operation, and high purity can be achieved.

Active Publication Date: 2009-12-09
河北远征禾木药业有限公司
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  • Abstract
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Problems solved by technology

The purity of the product obtained by this method is greatly improved compared with US4675330 (HPLC detection reaches more than 90%), but its purity still cannot be used as medicine, and its reactant is a turbid liquid low-temperature reaction, and the requirements for stirring and refrigeration are relatively high. high
[0011] There is currently no relevant patent in China

Method used

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  • Preparation method of valnemulin and hydrochloride thereof
  • Preparation method of valnemulin and hydrochloride thereof
  • Preparation method of valnemulin and hydrochloride thereof

Examples

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Embodiment Construction

[0037] The present invention will be further described below in conjunction with the examples, but not as a limitation of the present invention.

[0038] The overall process steps and process conditions of the present embodiment are as follows:

[0039] Preparation of hydrochloric acid ((2-((R)-2-amino-3-methylbutyrylamino)-1,1-dimethylethyl)mercapto)acetic acid, (3aS, 4R, 5S, 6S, 8R, 9R ,9aR,10R)-octahydro-5,8-dihydroxy-4,6,9,10-tetramethyl-6-vinyl-3a,9-propane-3aH-cyclopentacyclooctene-1(4H )-keto-8-ester (warnemulin hydrochloride).

[0040] In a 500ml four-neck flask equipped with electric stirring, a condenser and a thermometer, the hydroxydane salt of D-valine (11.36g, 44.79mmol) was added to 140ml of tetrahydrofuran, and stirred to make the hydroxydung salt of D-valine Suspend the salt solid, drop the temperature to 0-5°C and add triethylamine dropwise (at a rate of 3ml / min) until the reaction solution is clear, and about 10ml of triethylamine is used up. Keep the sti...

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Abstract

The invention belongs to preparation of antibiotic, in particular to preparation method of Valnemulin and hydrochloride thereof.D-hydroxy valine Dane salt is added into more than ten weight of tetrahydrofuran and is suspended by stirring at 0-20 DEG C, and triethylamine, N, N-dimethyl formamide (acetamide) and N-methyl morpholine are added until reaction liquid is clear; methyl (ethyl) chloroformate molar weight of which is not more than that of D-hydroxy valine Dane salt is added; (2-amino-1, 1-dimethyl ethyl) mercaptoacetic acid, (3aS, 4R, 5S, 6S, 8R, 9R, 9aR, 10R)-octohydrogen-5, 8-dyhydroxy-4, 6, 9,10-tetramethyl-6-ethenyl-3a, 9-propane-3aH-cyclopentene (cyclooctene)-1(4H)-keto-8-ester the molar weight of which is not more than that of D-hydroxy valine Dane salt is dissolved in equal mass of tetrahydrofuran, the reaction liquid is dripped in and stirred at 0-10 DEG C, and reaction is carried out for 2-5h at 0-20 DEG C; the organic solvent is removed, the residue is added with water and hydrochloric acid is used for adjusting pH value, heating up, stirring and decontaminating are carried out, and the filtration is freeze dried to obtain Valnemulin hydrochloride. The invention solves the problems of low purity and high reaction condition of the existing product and has the advantages of simple technology and high product purity.

Description

Technical field [0001] The invention belongs to the preparation of antibiotics, in particular to a preparation method of warnemulin and its hydrochloride. Background technique [0002] In the prior art, a large number of human antibiotics are used for animal breeding without research and scientific verification, so that the drug resistance of pathogenic bacteria is increasing day by day, the drug efficacy is rapidly declining, and the service life of the drug is shortened. Force people to have to increase the use concentration of antibiotic again and again or give up the antibiotic kind that once had very good effect, because there is the reason of misuse and non-standard medication in the livestock and poultry breeding process. Drug residues in animal products pose a direct threat to human health, causing people to pay attention to the "food safety" issue. The selection of animal health products in the world has tended to favor the use of broad-spectrum, high-efficiency, l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/20
Inventor 刘波李金明杨芳岳永波刘海亮
Owner 河北远征禾木药业有限公司
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