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Preparation method and applications of dehydro-lincomycin-free lincomycin hydrochloride

A technology of lincomycin hydrochloride and hydrolincomycin, which is applied in the field of medicine to achieve the effect of reducing drug impurities and improving drug quality

Active Publication Date: 2013-03-13
GUANGZHOU BAIYUSN TIANXIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] After searching, there is no patent or literature report on the method of removing or reducing dehydrolincomycin

Method used

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  • Preparation method and applications of dehydro-lincomycin-free lincomycin hydrochloride
  • Preparation method and applications of dehydro-lincomycin-free lincomycin hydrochloride
  • Preparation method and applications of dehydro-lincomycin-free lincomycin hydrochloride

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Embodiment 1

[0033] Dissolve 30g of lincomycin hydrochloride containing dehydrolincomycin in 40ml of water, add 0.3g of catalyst palladium carbon, pass in hydrogen and keep the pressure at 0.3MPa, stir for 25h, filter to remove carbon, and use 5ml of water and 40ml of acetone Combine the filtrate and the carbon washing liquid, stir and add 660ml of acetone dropwise at the same time, after the addition, cool down to below 10°C and stir for 1h, collect the crystals by filtration, and dry in vacuum at 50°C.

[0034] Lincomycin hydrochloride before and after preparation by the preparation method of the present invention, the illustrations are shown in figure 1 , figure 2 . It can be seen that the lincomycin hydrochloride prepared by the preparation method of the present invention does not contain dehydrolincomycin.

Embodiment 2

[0036] Dissolve 30g of lincomycin hydrochloride containing dehydrolincomycin in 40ml of water and 10ml of ethanol, add 1.5g of catalyst palladium carbon, continuously and slowly feed hydrogen, and stir for 5h, filter to remove carbon, and use 5ml of water Wash the carbon with a mixed solution of 50ml of acetone, combine the filtrate and the carbon washing solution, stir and add 610ml of acetone dropwise at the same time, after the addition, cool down to below 10°C and stir for 1h, collect the crystals by filtration, and vacuum dry at 50°C.

Embodiment 3

[0038] Dissolve 30g of lincomycin hydrochloride containing dehydrolincomycin in 40ml of water and 40ml of methanol, add 3.0g of catalyst palladium carbon, feed hydrogen and keep the pressure at 0.4MPa, stir for 1h, filter to remove carbon, and use 5ml Wash the carbon with a mixed solution of water and 40ml of acetone, combine the filtrate and the carbon washing liquid, stir and add 660ml of acetone dropwise at the same time, after the addition, cool down to below 10°C and stir for 1h, collect the crystals by filtration, and dry in vacuum at 50°C.

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Abstract

The invention relates to a preparation method and applications of dehydro-lincomycin-free lincomycin hydrochloride, which belong to the field of medical technologies. The preparation method disclosed by the invention comprises the following steps: dissolving dehydro-lincomycin-containing lincomycin hydrochloride serving as a raw material into water or an aqueous alcohol solution; adding palladium on carbon accounting for 1 / 10-1 / 200 of the amount of the raw material, and simultaneously stirring and introducing hydrogen into the obtained mixture to react for 1-48 hours, so that dehydro-lincomycin is all reacted to generate lincomycin; and crystallizing lincomycin. According to the preparation method, dehydro-lincomycin in lincomycin hydrochloride has a chemical reaction to generate lincomycin hydrochloride, so that dehydro-lincomycin in the raw material is completely removed; and the raw material can be used for preparing a dehydro-lincomycin-free lincomycin hydrochloride preparation, reducing the impurities in pharmaceutical products, and improving the quality of pharmaceutical products.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to lincomycin hydrochloride without dehydrolincomycin, a preparation method and application thereof. Background technique [0002] Lincomycin hydrochloride, 6-(1-methyl-trans-4-propyl-L-2-pyrrolidinecarboxamido)-1-thio-6,8-dideoxy-D-erythro-α -D-galactooctylactopyranoside hydrochloride-hydrate, the structural formula is shown in formula 1. [0003] [0004] Formula 1 Lincomycin Hydrochloride [0005] This product has a good effect on Gram-positive cocci, especially for anaerobic bacteria, Staphylococcus aureus and pneumococcus. Clinically, it is mainly used for various infections caused by sensitive bacteria, such as pneumonia, meningitis, endocarditis, cellulitis, tonsillitis, osteomyelitis and urinary system infection. [0006] Lincomycin hydrochloride mainly contains impurities lincomycin B, α-amide isomers, and dehydrolincomycin. Since the structure of dehydrolinco...

Claims

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Application Information

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IPC IPC(8): C07H15/16C07H1/06A61K31/7056A61P31/04
Inventor 谭胜连文青司徒小燕闵翠娥傅红燕陆媛郭泽彬
Owner GUANGZHOU BAIYUSN TIANXIN PHARMA
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