Method for refining and preparing erythromycin thiocyanate

A technology of erythromycin thiocyanate and its refining method, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., which can solve the problems of increased production costs, loss of erythromycin components, etc., and achieve solvent cost saving , simplification of process steps and huge economic benefits

Active Publication Date: 2013-09-04
SHANGHAI RECOM BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, when acetone is used as a solvent, water and acetone have a certain miscibility ratio, and while impurities are taken away through the water layer, part of the erythromycin component in the solution is also lost; not only that, the subsequent generation of erythromycin thiocyanate The required thiocyanate is also dissolved in water. Therefore, the separation of the water layer will also take away a large part of thiocyanate. Later, when erythromycin thiocyanate is salted and crystallized, it is necessary to replenish the lost sulfur The amount of cyanate, resulting in increased production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] The refining method of embodiment 1 erythromycin thiocyanate of the present invention

[0051] Crude erythromycin thiocyanate wet product (water content 30%, erythromycin titer 580 units / mg; HPLC external standard method detection, dry product containing 73% erythromycin A, containing 2.8% erythromycin B, containing 3% erythromycin C, containing 3% erythromycin E), adding methanol (3 liters of methanol per billion units of erythromycin), adjusting the pH to 9.5 with 20% sodium hydroxide solution, Convert erythromycin thiocyanate into erythromycin base, remove insoluble matter by filtration, add 20% sodium thiocyanate solution (0.4 mole sodium thiocyanate per 1 mole erythromycin), and use 50% glacial acetic acid solution Adjust the pH to 7.5, add purified water to 1 times the volume of the solution, control the crystallization temperature at 25-30°C, stir slowly for 10 minutes, then let it stand for 1 hour, filter to obtain the wet product of erythromycin thiocyanate, an...

Embodiment 2

[0054] The refining method of embodiment 2 erythromycin thiocyanate of the present invention

[0055] Get 1 kilogram of erythromycin thiocyanate crude product (water content 30%, erythromycin potency is 580 units / mg; HPLC external standard method detects, contains 73% erythromycin A in terms of dry product, contains 2.8% erythromycin A erythromycin B, containing 3% erythromycin C, containing 3% erythromycin E), adding ethanol (2.5 liters of ethanol per billion units of erythromycin), stirring, and adjusting the pH to 10 with 20% sodium hydroxide solution , and heated to 40±3°C, centrifuged to remove insoluble matter, washed the filter cake with ethanol (0.2 liter of ethanol for every billion units of erythromycin), combined the washing liquid and filtrate, added 100 ml of water, and raised the temperature to 45±3 ℃, add 40% sodium thiocyanate solution (0.9 moles of sodium thiocyanate is added to 1 mole of erythromycin), add 20% aqueous acetic acid to adjust the pH to 7.3, filt...

Embodiment 3

[0056] Embodiment 3 The refining method of erythromycin thiocyanate of the present invention

[0057] 20 kg of crude erythromycin thiocyanate (water content 30%, erythromycin titer 580 units / mg; HPLC external standard method detection, dry product contains 73% erythromycin A, containing 2.8% erythromycin B, containing 3% erythromycin C, containing 3% erythromycin E), add 99% methanol (add 2.5 liters of methanol for every billion units of erythromycin) and stir, add 30% sodium hydroxide solution to adjust pH to 9.6, heat up to 35°C and stir, remove insoluble matter by centrifugation in a butterfly centrifuge, wash the filter cake with methanol (wash with 0.1 liter of methanol for every billion units of erythromycin fed), combine the filtrate and washing liquid, and heat up to 35 ℃, add 40% sodium thiocyanate solution (0.3 moles of sodium thiocyanate per 1 mole of erythromycin), slowly add glacial acetic acid to pH=7.1, cool down to 25±3℃, add 0.6 times the amount of methanol P...

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PUM

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Abstract

The invention provides a method for refining erythromycin thiocyanate, which comprises the following steps: (1) fetching erythromycin thiocyanate crude product, dissolving in a solvent, treating with alkali, removing insoluble substances, adding thiocyanate, adding acid for adjusting pH to 5.5-8.3; (2) precipitating solid, washing, drying and obtaining the erythromycin thiocyanate finished product; wherein, the solvent in the step (1) is methanol, ethanol or isopropanol; Or, the solvent is a mixed solvent containing more than two ingredients among methanol, ethanol, isopropanol, water, acetone, dichloromethane, ethyl acetate and butyl acetate; in the mixed solvent, the contents of the methanol, ethanol or isopropanol are above 30% w / w. The invention also provides a preparation method of erythromycin thiocyanate. The invention overcomes the technology prejudice that the mixing and dissolving of solvent and water can not reduce the erythromycin impurity, and not only the purity and the yield of the erythromycin thiocyanate finished product are not reduced, but also the solvent cost is substantially saved and the technology step is simplified.

Description

technical field [0001] The invention relates to a refining and preparation method of erythromycin thiocyanate. Background technique [0002] Erythromycin thiocyanate (referred to as sulfur red) is the thiocyanate of erythromycin. Initially, erythromycin thiocyanate was a veterinary drug. With the development and application of semi-synthetic antibiotics, erythromycin thiocyanate erythromycin oxime can be synthesized to obtain clarithromycin, roxithromycin and azithromycin. In recent years, the demand for the three semi-synthetic erythromycins of clarithromycin, roxithromycin and azithromycin has risen rapidly in domestic and foreign markets, and the demand for erythromycin thiocyanate as a raw material for their synthesis is also on the rise. The main active ingredient of erythromycin is erythromycin A, and the impurity components mainly include erythromycin B, erythromycin C, erythromycin E, erythromycin F, etc. The impurity groups obtained from different strains and diffe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 刘革新张翔邹太平滕正华梁隆程志鹏刘思川王利春沈鑫
Owner SHANGHAI RECOM BIOTECHNOLOGY CO LTD
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