Method for preparing oxytetracycline hydrochloride

A technology of oxytetracycline hydrochloride and oxytetracycline hydrochloride, which is applied in the field of preparation of oxytetracycline hydrochloride, can solve the problems of excessive residue, difficulty in effective control of methanol content, and low content, and achieve the effect of high yield

Active Publication Date: 2010-12-15
扬州联博药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In its preparation process, if the preparation method is improper and the process conditions are not good, it is difficult to effectively control the methanol content in the finished product, and it is easy to cause the residue to exceed the standard and the content is low, which does not meet the requirements of the Pharmacopoeia. Therefore, methanol residue often becomes a problem for hydrochloric acid Oxytetracycline preparation is a big problem. Therefore, it is of great practical significance to study a method for preparing oxytetracycline hydrochloride whose quality meets the pharmacopoeia standard and whose residual solvent meets the requirements of ICH.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]Put 300g of oxytetracycline, 1800ml of methanol, and 25.5ml of methanol hydrochloride into the reactor in sequence, stir, heat to 48°C to dissolve all the oxytetracycline, add 3g of activated carbon, continue to heat up to 55°C, stir for 15 minutes, filter, and cool the filtrate To 26°C, add 30ml of dry HCL under stirring, gradually lower the temperature to 3°C at a speed of 45 rpm, continue to stir at this speed for 4 hours, filter, rinse the filter cake with 100ml of cold methanol, continue to filter until dry, wet product Pulverize, sieve, sieve hole 0.212mm, air-dry the loose granules after sieving, gas preheating temperature 120 ℃, air velocity 25m / s, get oxytetracycline hydrochloride 286.5g, productive rate 95.5%, each quality The indicators meet the standards of the Pharmacopoeia of the People's Republic of China, the United States Pharmacopoeia, the British Pharmacopoeia and the European Pharmacopoeia, and the content is in accordance with the Pharmacopoeia of the...

Embodiment 2

[0032] Put 300g of oxytetracycline, 1200ml of methanol, and 27ml of methanol hydrochloride into the reactor in turn, stir, heat to 48°C to dissolve all the oxytetracycline, add 3.5g of activated carbon, continue to heat up to 54°C, stir for 15 minutes, filter, and cool the filtrate To 28°C, add 30g of dry HCL under stirring, gradually cool down to 3°C at a speed of 50 rpm, continue to stir at this speed for 4 hours, filter, rinse the filter cake with 100ml of cold methanol, continue to filter until dry, wet product Pulverize, sieve, sieve hole 0.300mm, air-dry the loose granules after sieving, gas preheating temperature 100 ℃, air velocity 20m / s, get oxytetracycline hydrochloride 289.5g, productive rate 96.5%, each quality The indicators meet the standards of the Pharmacopoeia of the People's Republic of China, the United States Pharmacopoeia, the British Pharmacopoeia and the European Pharmacopoeia, and the content is in accordance with the Pharmacopoeia of the People's Republ...

Embodiment 3

[0034] Put 300g of oxytetracycline, 1200ml of methanol, and 27ml of methanol hydrochloride into the reactor in turn, stir, heat to 48°C to dissolve all the oxytetracycline, add 4g of activated carbon, continue to heat up to 55°C, stir for 15 minutes, filter, and cool the filtrate to 28°C, pour 33g of dry HCL under stirring, gradually cool down to 3°C at a speed of 45 rpm, continue stirring at this speed for 4 hours, filter, rinse the filter cake with 100ml of cold methanol, continue to filter until dry, and crush the wet product , sieved, sieve hole 0.300mm, the loose granules after sieving are carried out airflow drying, gas preheating temperature 105 ℃, air velocity 30m / s, get oxytetracycline hydrochloride 290.0g, yield 96.7%, each quality index Conforms to the Pharmacopoeia of the People's Republic of China, the United States Pharmacopoeia, the British Pharmacopoeia and the European Pharmacopoeia, and the content is in accordance with the Pharmacopoeia of the People's Republ...

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Abstract

The invention provides a method for preparing oxytetracycline hydrochloride. In the method, oxytetracycline is used as an initiative raw material, hydrochloric acid and methanol are used as co-solvents, and active carbon is used for decolorizing. A finished product is obtained by salt formation under the action of dry HCL, dynamical stirring, cooling and crystallization, crushing and screening of a wet product and airflow drying. The oxytetracycline hydrochloride prepared by the preparation method accords with the standards of Chinese Pharmacopoeia, United States Pharmacopeia, British Pharmacopoeia and European Pharmacopoeia, the methanol residue is superior to ICH requirement, and the yield reaches over 95.5 percent.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a preparation method of oxytetracycline hydrochloride. Background technique [0002] Oxytetracycline hydrochloride, also known as oxytetracycline hydrochloride, oxytetracycline hydrochloride, or oxytetracycline hydrochloride, is an antibiotic widely used in humans and animals, and is clinically used to treat various diseases, such as rickettsiasis, including Epidemic typhus, endemic typhus, scrub typhus; infection caused by Mycoplasma pneumoniae; chlamydial infection, including psittacosis, venereal lymphoid edema, nonspecific urethritis, salpingitis, and trachoma; relapsing fever; Brucella disease; cholera; plague and tularemia, etc. The dosage forms of oxytetracycline hydrochloride are tablets, capsules, powders, eye drops and ointments. [0003] The Pharmacopoeia of the People's Republic of China, the United States Pharmacopoeia, the British Pharmacopoeia and the European ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/26C07C231/12C07C231/24
Inventor 陆波苏令
Owner 扬州联博药业有限公司
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