Refining method and preparation method of 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 loss of erythromycin components and increased production costs, and save solvent costs , simplified process steps, and good application prospects

Inactive Publication Date: 2013-02-06
YILI CHUANNING BIOTECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 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

[0046] The refining method of embodiment 1 erythromycin thiocyanate of the present invention

[0047] 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, and ...

Embodiment 2

[0050] The refining method of embodiment 2 erythromycin thiocyanate of the present invention

[0051] 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 warm up to 40±3°C, filter to remove insoluble matter, wash the filter cake with ethanol (wash with 0.2 liter of ethanol for every billion units of erythromycin), combine the washing liquid and filtrate, add 100 ml of water, and heat up to 45±3°C , add 40% sodium thiocyanate solution (0.9 moles of sodium thiocyanate per 1 mole of erythromycin), add 20% aqueous acetic acid to adjust the pH to 7.3, filter to obtain the wet ...

Embodiment 3

[0052] The refining method of embodiment 3 erythromycin thiocyanate of the present invention

[0053] 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, filter, 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, heat up to 35°C, add 40% thiocyanic acid Sodium solution (add 0.3 moles of sodium thiocyanate for every mole of erythromycin), slowly add glacial acetic acid to pH = 7.1, cool down to 25±3°C, add purified water according to 0.6 times the amount of methanol, and then cool down to 1...

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PUM

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Abstract

The invention provides a refining method of erythromycin thiocyanate and a preparation method of the erythromycin thiocyanate. The refining method of the erythromycin thiocyanate comprises the following steps of: (1) dissolving an erythromycin thiocyanate coarse product in a solvent, performing alkaline treatment, filtering off insoluble matters, adding thiocyanate and then adding acid to regulate pH (Potential of Hydrogen) to be 5.5-8.3; and (2) separating a solid matter out, washing and drying to obtain an erythromycin thiocyanate finished product, wherein the solvent in the step (1) is methanol, ethanol or isopropyl alcohol; or the solvent is mixed solvent of more than two of methanol, ethanol, isopropyl alcohol, water, acetone, dichloroethane, ethyl acetate and butyl acetate; and the content of the methanol, the ethanol or the isopropyl alcohol is over 30 percent w/w in the mixed solvent. According to the refining method and the preparation method of the erythromycin thiocyanate, the technical bias that the erythromycin impurity cannot be reduced because of mixing of the solvent and the water existing in the conventional method is overcome, the purity and the yield of the erythromycin thiocyanate finished product are not reduced, the solvent cost is also obviously saved, and the technological steps are also obviously 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): C07H17/08C07H1/06C07H1/00
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 YILI CHUANNING BIOTECH CO
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