Method for producing large-grain oxytetracycline hydrochloride

A technology of oxytetracycline hydrochloride and large particles, which is applied in the field of producing large particles of oxytetracycline hydrochloride, which can solve the problems of unsatisfactory use requirements, unreliable bonding of small crystals, and low bulk density, and achieve high bulk density and good fluidity , the effect of increasing yield

Active Publication Date: 2017-08-04
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

The crystal form of oxytetracycline hydrochloride prepared by this process belongs to the needle-like single crystal. Even if large polycrystalline particles are formed, because the small crystals are not firmly bonded, they are easy to become small single crystals, and the final product is a fine crystal powder with poor fluidity. , the bulk density is relatively low, 0.3-0.4g / mL
However, the bulk density required by some customers of oxytetracycline hydrochloride at home and abroad is greater than 0.4g / mL. Therefore, the existing technology cannot meet the use requirements.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The method for existing production oxytetracycline hydrochloride, step is as follows:

[0023] 1) Add 6.07mL of methanolic hydrogen chloride solution (acidity: 33%, volume ratio) into 400mL of methanol, raise the temperature to 40°C at the same time, add 80g of oxytetracycline, stir until completely dissolved, and obtain a mixed solution;

[0024] 2) Add 0.4g of activated carbon to the mixed solution in step 1), stir for 10min, then add 0.8g of diatomaceous earth, filter to obtain the filtrate.

[0025] 3) Add 16g of hydrogen chloride methanol solution to the filtrate in step 2), stir for 5min, crystals precipitate, cool down to 5°C, let stand for 3h, filter to obtain 400mL of production mother liquor (for standby), the filter cake is washed with methanol solution at 0°C, Get trendy.

[0026] 4) Dry the wet product in step 3) in a vacuum drying oven at 88°C for 4 hours to obtain 74g of dry product of oxytetracycline hydrochloride for the first application.

[0027] 5)...

Embodiment 2

[0029] The method for producing large particle oxytetracycline hydrochloride of the present invention, step is as follows:

[0030] 1) Add 607mL of methanolic hydrogen chloride solution into 40L of methanol, raise the temperature to 40°C at the same time, add 8Kg of oxytetracycline, and stir until completely dissolved to obtain a mixed solution.

[0031] 2) Add 40g of activated carbon to the mixed solution in step 1), stir for 10 minutes, then add 80g of diatomaceous earth, filter to obtain the filtrate.

[0032] 3) Add 40L of mother liquor (the mother liquor obtained in Example 1 or the mother liquor produced in this step) to the filtrate to obtain a mixed solution, stir and raise the temperature to 40°C, add 1.7Kg hydrogen chloride methanol solution to the mixed solution, stir for 5min, and crystals precipitate out. Cool down to 5°C, let it stand for 3 hours, and filter to obtain 80L of production mother liquor (retained). The filter cake is washed with methanol solution at ...

Embodiment 3

[0036] The method for producing large particle oxytetracycline hydrochloride of the present invention, step is as follows:

[0037] 1) Add 5L of methanolic hydrogen chloride solution into 400L of methanol, raise the temperature to 40°C at the same time, add 80Kg of oxytetracycline, and stir until completely dissolved to obtain a mixed solution.

[0038] 2) Add 400g of activated carbon to the mixed solution in step 1), stir for 10 minutes, then add 800g of diatomaceous earth, filter to obtain the filtrate.

[0039] 3) Add 400L mother liquor (the mother liquor obtained in Example 1, the mother liquor obtained in Example 2, or the mother liquor produced in this step) to the filtrate to obtain a mixed solution, stir and heat up to 45°C, add 16Kg hydrogen chloride methanol solution to the mixed solution, Stir for 5 minutes, crystals are precipitated, lower the temperature to 5°C, let stand for 3h, filter to obtain 800L of production mother liquor (reserve), and wash the filter cake...

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PUM

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Abstract

The invention discloses a method for producing large-grain oxytetracycline hydrochloride. The method comprises the steps of dissolving, activated carbon decolorization treatment, crystallization and drying; and during batch operation, a mother liquor generated in the previous process is added to a filtrate in the crystallization step and the mother liquor generated in the crystallization step is further used in the next process. According to the method for producing the large-grain oxytetracycline hydrochloride, 1-3 times of mother liquor (produced from the previous round) is added to the filtrate before acid-adding salt formation on the basis of not changing the original technological process, so that an oxytetracycline hydrochloride crude drug which is good in mobility and high in bulk density and meets the requirements of customers can be produced while the yield of the oxytetracycline hydrochloride is effectively increased; and the oxytetracycline hydrochloride crude drug has good practicability.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, in particular to a method for producing large particle oxytetracycline hydrochloride. Background technique [0002] Oxytetracycline hydrochloride, also known as oxytetracycline hydrochloride and oxytetracycline hydrochloride, is a widely used antibiotic, clinically used in the treatment of various diseases, such as rickettsial disease; infection caused by Mycoplasma pneumoniae; chlamydia infection, etc. . The dosage forms of oxytetracycline hydrochloride clinically used include tablets, capsules, powders, ointments, etc. [0003] The technique of producing oxytetracycline hydrochloride crude drug at present is that oxytetracycline is dissolved in the anhydrous methanol that contains certain acidity, adds activated carbon and carries out decolorization treatment, then filters, and obtains filtrate, and the mass volume ratio of oxytetracycline and methyl alcohol in the filtrate is 1:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C237/26
Inventor 黄忠明章留留余贞宇
Owner 扬州联博药业有限公司
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