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A kind of preparation method of erythromycin thiocyanate

A technology of erythromycin thiocyanate and erythromycin, which is applied in the directions of sugar derivatives and organic chemistry, can solve the problems of many impurities and low purity, and achieve the effects of high purity, excellent selectivity and low boiling point.

Active Publication Date: 2016-03-02
HEC PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The prior art has the following disadvantages: the product erythromycin thiocyanate A obtained by the prior art is less than 78%, and because the purity is low and there are too many impurities, it cannot be used as a starting material to synthesize azithromycin and carat that meet European standards and American standards. Derivatives such as mycin

Method used

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  • A kind of preparation method of erythromycin thiocyanate
  • A kind of preparation method of erythromycin thiocyanate
  • A kind of preparation method of erythromycin thiocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Take 100g of crude erythromycin, add 600mL of acetone, place in a water bath and heat to 35°C, adjust the pH to 8.5, filter to obtain the filtrate, keep the filtrate at 35°C, add sodium thiocyanate, the molar ratio is 2:1, After stirring to make it dissolve, use acetic acid to adjust the pH of the solution to 6.0, slowly cool down to 10°C, keep warm for about 15 minutes, then centrifuge, rinse with 100mL purified water, crush and dry to obtain erythromycin thiocyanate, the main component of which is red The content of mycin A is 85.1% (detected by HPLC method, calculated as dry product).

Embodiment 2

[0049] Take 150g of crude erythromycin thiocyanate, add 600mL of acetone, place in a water bath and heat to 45°C, adjust the pH to 10.0, filter to obtain the filtrate, keep the filtrate at 45°C, add potassium thiocyanate, the molar ratio of addition is 0.2 : 1, stir to make it dissolve, use dilute hydrochloric acid to adjust the pH of the solution to 7.5, slowly cool down to 0°C, keep warm for about 15 minutes, centrifuge, use 100mL purified water to rinse, pulverize, and dry to obtain erythromycin thiocyanate. Its main component, erythromycin A, has a content of 84.7% (detected by HPLC method, calculated as dry product).

Embodiment 3

[0051] Take 150g of crude erythromycin lactate, add 600mL of acetone, place in a water bath and heat to 40°C, adjust the pH to 9.0, filter to obtain the filtrate, keep the filtrate at 45°C, add ammonium thiocyanate, the molar ratio of addition is 2:1 , stir to make it dissolve, use dilute hydrochloric acid to adjust the pH of the solution to 7.5, slowly cool down to 5°C, keep it warm for about 15 minutes, then centrifuge, rinse with 100mL of purified water, pulverize and dry to obtain erythromycin thiocyanate. The content of component erythromycin A is 84.9% (detected by HPLC method, calculated as dry product).

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Abstract

Disclosed is a preparation process of erythromycin thiocyanate, which belongs to the pharmaceutical field. The preparation process provided by the invention uses erythromycin or its salt(s) as raw material(s), dissolves it / them in acetone or the mixed solvent containing acetone and obtains erythromycin thiocyanate rich in erythromycin thiocyanate A as the main component and low in the content of impurities. Said erythromycin thiocyanate could be used as the raw material for preparing Azithromycin and Clarithromycin, which meets to the standards made by European Union and US.

Description

[0001] This application claims the priority of the Chinese patent application filed on August 26, 2011 with the application number of 201110248968.2 and the invention titled "A method for preparing erythromycin thiocyanate", the entire contents of which are incorporated by reference in this application. technical field [0002] The invention relates to the field of pharmacy, in particular to a preparation method of erythromycin thiocyanate. Background technique [0003] Currently, the three leading drugs in the global anti-infective drug market are cephalosporins / semi-synthetic penicillins, fluoroquinolones and macrolides, which together account for 80% of the anti-infective drug market share. Among them, macrolide antibiotics led by third-generation erythromycin (such as azithromycin, clarithromycin and roxithromycin) have steadily increased their share in the international market in recent years. At present, my country has become the world's largest producer of macrolide ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08
CPCC07H17/08C07D407/14
Inventor 熊辉赵科义邓肇政
Owner HEC PHARM CO LTD
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