Method for preparing clindamycin phosphate

A technology of clindamycin phosphate and dehydroclindamycin is applied in the field of medicine to achieve the effect of reducing the content of impurities and improving the quality of medicines

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

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Problems solved by technology

[0014] After searching, there are no relevant patents and literature reports on removing or reducing dehydroclindamycin phosphate

Method used

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  • Method for preparing clindamycin phosphate
  • Method for preparing clindamycin phosphate
  • Method for preparing clindamycin phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Add 10 g of clindamycin phosphate containing dehydroclindamycin phosphate to 100 ml of water, stir to dissolve, add 2.0 g of catalyst palladium carbon after dissolving, pass in hydrogen and keep the hydrogen pressure at 0.4 Mpa, and continue stirring for 1 h. Filter and wash the carbon with a mixed solution of 5ml of water and 40ml of absolute ethanol, combine the filtrate and the carbon washing solution, and add 60ml of absolute ethanol, rotary evaporate at 60°C until about 40ml of liquid remains, then add 50ml of absolute ethanol to it, Continue rotary evaporation at 60°C until a small amount of crystals precipitate, take it out and stir, add 100ml of absolute ethanol dropwise at the same time, cool down to above 10°C for 1 hour, collect crystals by filtration, and vacuum dry at 50°C.

Embodiment 2

[0031] Add 10 g of clindamycin phosphate containing dehydroclindamycin phosphate to a mixed solution of 100 ml water and 20 ml ethanol, stir and dissolve, add catalyst palladium carbon 0.5 g after dissolving, continue to feed hydrogen slowly, and Stir the reaction for 24 hours, filter and wash the carbon with a mixed solution of 5ml of water and 30ml of absolute ethanol, combine the filtrate and the carbon washing solution, and add 60ml of absolute ethanol, and rotary evaporate at 60°C until about 40ml of liquid remains, and then add no Water and ethanol 60ml, continue to rotary evaporate at 60°C until a small amount of crystals are precipitated, take it out and stir, at the same time add 100ml of absolute ethanol dropwise, cool to above 10°C for 1 hour, collect crystals by filtration, and vacuum dry at 50°C.

Embodiment 3

[0033] Add 10 g of clindamycin phosphate containing dehydroclindamycin phosphate to a mixed solution of 100 ml water and 40 ml methanol, stir and dissolve, add catalyst palladium carbon 1.0 g after dissolving, continuously and slowly feed hydrogen, and Stir the reaction for 3 hours, filter and wash the carbon with a mixed solution of 5ml of water and 30ml of absolute ethanol, combine the filtrate and the carbon washing solution, add 60ml of absolute ethanol, and rotate to evaporate at 60°C until about 40ml of liquid remains, then add no Water and ethanol 60ml, continue to rotary evaporate at 60°C until a small amount of crystals are precipitated, take it out and stir, at the same time add 100ml of absolute ethanol dropwise, cool to above 10°C for 1 hour, collect crystals by filtration, and vacuum dry at 50°C.

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Abstract

The invention relates to a method for preparing clindamycin phosphate, belonging to the field of medicine technologies. According to the method, clindamycin phosphate containing dehydro-clindamycin phosphate is taken as a raw material and dissolved into water or water-containing alcoholic liquid, 1/5-1/100 of the raw material amount of palladium carbon is added, hydrogen is introduced to react for 1-48 hours while stirring, the dehydro-clindamycin phosphate is enabled to fully produce the clindamycin phosphate, and then crystallization is carried out. The method has the advantages that the dehydro-clindamycin phosphate can be enabled to fully produce the clindamycin phosphate, so that the content of impurities in drugs is reduced, and the quality of the drugs is improved.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a high-purity clindamycin phosphate and a preparation method thereof. Background technique [0002] Clindamycin phosphate is an antibiotic semi-synthesized from lincomycin, and its structure is shown in formula 1: [0003] [0004] Formula 1 Clindamycin Phosphate [0005] Clindamycin phosphate is a prodrug, which has no antibacterial activity in vitro. After entering the human body, it is rapidly hydrolyzed into clindamycin, and achieves antibacterial effect by inhibiting the synthesis of bacterial cell wall proteins. Clinically, it is mainly used for various infections caused by anaerobic bacteria and Gram-positive aerobic bacteria, such as respiratory tract infection, urinary tract infection, bone and joint infection, pelvic infection, abdominal infection, skin and soft tissue infection caused by sensitive bacteria . [0006] According to the research on clindamycin phosph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/16C07H1/00A61K31/7056A61P31/04
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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