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
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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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