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Method for preparing clindamycin hydrochloride

A technology of clindamycin hydrochloride and lincomycin, which is applied to the preparation of lincosamide antibiotics clindamycin hydrochloride and the field of beta-lactam antibiotics, can solve the problems of high cost, low yield by weight in batches, Process complexity and other problems, to achieve the effect of improving quality, reducing equipment investment, and simplifying the process

Inactive Publication Date: 2012-10-03
ANHUI WANBEI PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the traditional process are: 1. The HCL-ethanol crystallization step is required, the process is complicated and the cost is high; 2. The weight yield of the batch is low, and the yield is about 88%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A. Add 45g of lincomycin according to the synthesis process of alcoholate for chlorination reaction to obtain 300ml of chloroform solution of clindamycin hydrochloride alcoholate, cool to 30°C, add 100ml of purified water, stir and wash for 30 minutes, let stand to separate out of the organic phase;

[0021] B. Add purified water to the washed organic phase at a volume ratio of 1:4, add concentrated hydrochloric acid dropwise at 30-35°C to adjust the pH value to 2, stir for 30 minutes, and let stand to separate layers;

[0022] C. Add activated carbon to decolorize the separated water phase at 30-35°C according to the mass ratio of 500:1 for 1 hour, and filter;

[0023] D. After the resin is adsorbed on the filtrate, wash with deionized water on the column for 24 hours, and the water consumption is 5 times the volume of the resin;

[0024] E. After washing with water, desorb with methanol with a mass concentration of more than 95%, and collect the analysis solution;

...

Embodiment 2

[0032] A. Add 50g of lincomycin according to the synthesis process of alcoholate for chlorination reaction to obtain 360ml of chloroform solution of clindamycin hydrochloride alcoholate, cool to 30°C, add 120ml of purified water, stir and wash for 30 minutes, let stand to separate out of the organic phase;

[0033] B. Add purified water to the washed organic phase at a volume ratio of 1:4, add concentrated hydrochloric acid dropwise at 30-35°C to adjust the pH value to 2.5, stir for 30 minutes, and let stand to separate layers;

[0034] C. Add activated carbon to decolorize the separated water phase at 30-35°C according to the mass ratio of 500:1 for 1 hour, and filter;

[0035] D. After resin adsorption on the filtrate, wash with deionized water on the column for 30 hours, and the water consumption is 7 times of the volume of the resin;

[0036] E. After washing with water, desorb with methanol with a mass concentration of more than 95%, and collect the analysis solution;

...

Embodiment 3

[0044] A. Add 50g of lincomycin according to the synthesis process of alcoholate for chlorination reaction to obtain 330ml of chloroform solution of clindamycin hydrochloride alcoholate, cool to 30°C, add 110ml of purified water, stir and wash for 30 minutes, let it stand for separation out of the organic phase;

[0045] B. Add purified water to the washed organic phase at a volume ratio of 1:4, add concentrated hydrochloric acid dropwise at 30-35°C to adjust the pH value to 3, stir for 30 minutes, and let stand to separate layers;

[0046] C. Add 3.0g of activated carbon to decolorize the separated water phase at 30-35°C according to the mass ratio of 500:1 for 1 hour, and filter;

[0047] D. After the resin is adsorbed on the filtrate, it is washed with deionized water for 28 hours, and the water consumption is 10 times of the volume of the resin;

[0048] E. After washing with water, desorb with methanol with a mass concentration of more than 95%, and collect the analysis ...

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PUM

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Abstract

The invention discloses a method for preparing clindamycin hydrochloride. The method comprises the following steps of: a) adding purified water into a chloroformic solution of clindamycin hydrochloride alcohol complex and washing; b) adding purified water into the washed organic phase, dripping hydrochloric acid to adjust PH value to be 2 to 3, standing and layering; c) adding activated carbon into a water phase obtained through separation and decoloring, and filtering; d) adsorbing filtrate by using a resin, and washing by using deionized water; e) desorbing by using methanol of which the mass concentration is more than 95 percent; f) concentrating a desorption solution under reduced pressure; g) adding acetone into concentrated dried materials, and stirring at the temperature of between 55 and 58 DEG C until the solution is clarified; h) dripping hydrochloric acid to adjust PH value to be 2 to 2.5; and i) reducing temperature to 0 to 5 DEG C, performing suction filtration under negative pressure to obtain web powder, washing by using iced acetone, and after suction filtration, drying to obtain the clindamycin hydrochloride. According to the method, the step of alcohol complex crystallization in the conventional process is eliminated; the process is simplified; production cost is reduced; and the weight yield and the quality of the whole batch of clindamycin hydrochloride are improved simultaneously.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy and relates to a β-lactam antibiotic, in particular to a preparation method of the lincosamide antibiotic clindamycin hydrochloride. technical background [0002] Clindamycin Hydrochloride (Clindamycin Hydrochloride) chemical name: 6-(1-methyl-trans-4-propyl-L-2-pyrrolidinecarboxamido)-1-thio-7(S)-chloro- 6,7,8-trideoxy-L-threo-α-D-galactopyranoside hydrochloride, a lincosamide antibiotic, is a 7-deoxy-7-chloro derivative of lincomycin Clindamycin was synthesized for the first time in 1966 by Magerlein et al. who replaced the 7th hydroxyl group in the lincomycin molecule with chlorine. It was first listed in the United States in the early 1970s by the American Upjohn Company, and then in the United Kingdom and other European countries. listed. Compared with lincomycin, clindamycin has a broad antibacterial spectrum and strong antibacterial activity. Its antibacterial activity is 4 to 8 times tha...

Claims

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Application Information

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IPC IPC(8): C07H15/16C07H1/00C07H1/06
Inventor 王幸杨平刘思远李为全刘瑞华
Owner ANHUI WANBEI PHARMA
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