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Crystallization method of clindamycin phosphate

A technology of clindamycin phosphate and crystallization, applied in the production field of clindamycin phosphate, can solve the problems of low crystallization yield and the like, and achieve the effects of high crystallization yield, improved purity, and not easy to agglomerate

Active Publication Date: 2013-07-10
XINYU PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical solution to be solved by the present invention is to provide a crystallization method of clindamycin phosphate, which solves the problem of low crystallization yield in the existing crystallization method of clindamycin phosphate

Method used

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  • Crystallization method of clindamycin phosphate

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Effect test

Embodiment 1

[0021] (1), in a 500ml spherical decolorizing tank, drop about 40g of clindamycin phosphate coarse powder (clindamycin hydrochloride obtained through esterification, hydrolysis, adsorption, and crude crystallization), add 64.8g of n-butanol and 80g of purified Water, stir and heat up to 78-80°C under water bath conditions, and keep the temperature constant for about 60 minutes;

[0022] (2), after the clindamycin phosphate coarse powder is fully dissolved, add 2g of activated carbon for decolorization, and filter while hot to remove insoluble impurities;

[0023] (3), the decolorizing liquid is pressed into a 500ml spherical crystallization tank through a fine filter, 64.8g of n-butanol is added, and when the clarified hot saturated solution of the gained is cooled to 60°C, it is vacuum concentrated, and the vacuum degree is greater than or equal to 0.09MPa. When the crystals are precipitated, stop the concentration, stir the solution at a speed of 100r / min, and keep the tempe...

Embodiment 2

[0026] (1), in a 1000ml spherical decolorization tank, drop about 80g of clindamycin phosphate coarse powder (clindamycin hydrochloride obtained through esterification, hydrolysis, adsorption, and crude crystallization), add 129.6g of n-butanol and 160g of purified Water, stir and heat up to 70-80°C in a water bath, and keep the temperature constant for about 60 minutes;

[0027] (2), after the clindamycin phosphate coarse powder is fully dissolved, add 4g of activated carbon for decolorization, and filter while hot to remove insoluble impurities;

[0028] (3) Press the decolorizing solution into a 1000ml spherical crystallization tank through a fine filter, add 129.6g of n-butanol, and when the resulting clear hot saturated solution is cooled to 60°C, slowly vacuum it to concentrate, when crystals are precipitated , stop the concentration, stir the solution at a speed of 100r / min, and keep the temperature at this temperature for 60min;

[0029] (4), then adjust the stirring ...

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Abstract

The invention discloses a crystallization method of clindamycin phosphate, comprising the following steps: firstly dissolving the clindamycin phosphate in n-butanol aqueous solution; then performing crystallization after decoloration, concentration and stepped temperature reduction to below 25 DEG C, filtering, washing, and drying to obtain the finished product. The crystallization method of the clindamycin phosphate of the invention has high crystallization yield, saves the time and reduces the cost; and the clindamycin phosphate finished product has high purity, good mobility and less possibility of agglomeration.

Description

technical field [0001] The invention relates to a production method of clindamycin phosphate, in particular to a crystallization method of clindamycin phosphate. Background technique [0002] Clindamycin Phosphate is an antibiotic drug, its chemical name is: methyl 6-(1-methyl-trans-4-propyl-L-2-pyrrolidinecarboxamido)-1-thio-7 (S)-Chloro-6,7,8-trideoxy-L-threo-a-D-galactopyranoside-2-phosphate. It has been listed in my country since 1970. Clindamycin phosphate is a chemically semi-synthesized clindamycin derivative, which has no antibacterial activity in vitro. After entering the body, it is rapidly hydrolyzed to clindamycin to exert its pharmacological effects. Its antibacterial spectrum, antibacterial activity and therapeutic effect are the same as clindamycin, but its fat solubility and permeability are better than clindamycin, and it can be administered orally, intramuscularly or intravenously. Compared with lincomycin, clindamycin phosphate has 4-8 times stronger an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/16C07H1/06
Inventor 夏守友刘伟孙冠中黄超
Owner XINYU PHARM CO LTD
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