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Preparation method for oxytetracycline hydrochloride

A technology of oxytetracycline hydrochloride and high-purity hydrochloric acid, which is used in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc.

Inactive Publication Date: 2015-04-15
内蒙古格林特制药有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The highest yield of this process is 85%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1 A kind of preparation method of oxytetracycline hydrochloride adopts the following steps:

[0012] (A) Dissolve 20 Kg of anhydrous calcium chloride in 750 L of methanol solvent, add 4 Kg of diatomaceous earth as a filter aid, stir, and filter the methanol solution to obtain a methanolic calcium chloride solution;

[0013] (B) First add 5 L of high-purity hydrochloric acid to the methanolic calcium chloride solution and stir evenly, then add 150 Kg of oxytetracycline base and stir to dissolve, then add 45 L of high-purity hydrochloric acid, cool down and crystallize to obtain oxytetracycline hydrochloride crystals;

[0014] (C) Put the crystals of oxytetracycline hydrochloride into a centrifuge, wash them with 200L methanol four times, centrifuge for 50 minutes after washing, and put the discharged materials into a boiling dryer to boil and dry, and gradually heat up to 65°C to keep warm 1 hour, then raise the temperature to 95°C and keep it warm for 20 minu...

Embodiment 2

[0016] Embodiment 2 A kind of preparation method of oxytetracycline hydrochloride adopts the following steps:

[0017] (A) Dissolve 30 Kg of anhydrous calcium chloride in 900 L of methanol solvent, add 6 Kg of diatomaceous earth as a filter aid at the same time, stir, and filter the methanol solution to obtain a methanolic calcium chloride solution;

[0018] (B) First add 6 L of high-purity hydrochloric acid to the methanolic calcium chloride solution and stir evenly, then add 180 Kg of oxytetracycline base to fully stir and dissolve, then add 70 L of high-purity hydrochloric acid, cool down and crystallize to obtain oxytetracycline hydrochloride crystals;

[0019] (C) Put the crystals of oxytetracycline hydrochloride into a centrifuge, wash them with 200L methanol four times, centrifuge for 50 minutes after washing, and put the discharged materials into a boiling dryer to boil and dry, and gradually heat up to 65°C to keep warm 1 hour, then raise the temperature to 95°C and k...

Embodiment 3

[0021] Embodiment 3 A kind of preparation method of oxytetracycline hydrochloride adopts the following steps:

[0022] (A) Dissolve 25 Kg of anhydrous calcium chloride in 800 L of methanol solvent, add 5 Kg of diatomaceous earth as a filter aid at the same time, stir, and filter the methanol solution to obtain methanol calcium chloride solution;

[0023] (B) First add 8 L of high-purity hydrochloric acid to the methanolic calcium chloride solution and stir evenly, then add 175 Kg of oxytetracycline base and stir to dissolve, then add 50 L of high-purity hydrochloric acid, cool down and crystallize to obtain oxytetracycline hydrochloride crystals;

[0024] (C) Put the crystals of oxytetracycline hydrochloride into a centrifuge, wash them with 200L methanol four times, centrifuge for 50 minutes after washing, and put the discharged materials into a boiling dryer to boil and dry, and gradually heat up to 65°C to keep warm 1 hour, then raise the temperature to 95°C and keep it war...

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PUM

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Abstract

The invention discloses a preparation method for oxytetracycline hydrochloride. The preparation method comprises the following steps: (A) dissolving 20-30 Kg of anhydrous calcium chloride into 750-900 L of methanol solvent, adding 4-6 Kg of diatomaceous earth to facilitate filtration at the same time, stirring, and filtering a methanol solution to obtain a methanol-calcium chloride solution; (B) adding 5-8 L of high-purity hydrochloric acid into the methanol-calcium chloride solution, uniformly stirring, then adding 150-180 Kgof oxytetracycline dihyclorate, fully stirring for dissolution, adding 45-70 L of high-purity hydrochloric acid, and performing cooling crystallization to obtain oxytetracycline hydrochloride crystals; (C) placing the oxytetracycline hydrochloride crystals into a centrifuge, leaching the oxytetracycline hydrochloride crystals for four times with 200 L of methanol, performing centrifugation for 50 minutes after leaching, discharging, and performing fluidized drying, and after drying, cooling and discharging to obtain a oxytetracycline hydrochloride finished product. According to the preparation method, the oxytetracycline hydrochloride yield can be stabilized to be about 94 percent.

Description

technical field [0001] The present invention relates to the preparation method of crude drug, specifically the preparation method of oxytetracycline hydrochloride. Background technique [0002] Oxytetracycline hydrochloride is an antibiotic raw material drug, English name: Oxytetracycline HCL, is a tetracycline antibiotic. Alias: Detetracycline, Oxytetracycline. This product is a broad-spectrum bacteriostatic agent, and many Rickettsia, Mycoplasma, Chlamydia, Spirochetes, Amoebas and some Plasmodium are also sensitive to this product. Enterococci are resistant to it. Others such as Actinomycetes, Bacillus anthracis, Listeria monocytogenes, Clostridium, Nocardia, Vibrio, Brucella, Campylobacter, Yersinia, etc. are sensitive to this product. The current domestic production process of oxytetracycline hydrochloride is as follows: Dissolve 23kg of anhydrous calcium chloride in 450kg of methanol containing 0.35% hydrogen chloride, add 100kg of oxytetracycline base, heat up to ...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/12
Inventor 胡志远孙洪峰赵一楠涂根顺徐思张士军杨春艳
Owner 内蒙古格林特制药有限责任公司
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