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A kind of preparation method of tetracycline hydrochloride

A technology of tetracycline hydrochloride and tetracycline, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., can solve problems such as increased production costs, urea consumption, yield loss, etc., and achieves reduction of production equipment and personnel. The effect of reducing and lowering production costs

Active Publication Date: 2017-12-22
NINGXIA QIYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of converting tetracycline into urea tetracycline, the method has yield loss, urea consumption, personnel wages, and causes the production cost of the product to increase.

Method used

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  • A kind of preparation method of tetracycline hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 100 g of tetracycline wet alkali with a water content of 15%. According to the ratio of tetracycline (dried): butanol = 1:5-6, measure 425ml of butanol at a temperature of 17°C. Mix and stir evenly, adjust with 30ml of concentrated hydrochloric acid, measure the solution with pH test paper in the range of pH=1.7~1.9, the solution is clear, and measure its potency unit to be 154501u / ml. Begin to heat up, with 30 minutes the solution temperature is raised to 51 ℃, continue to keep warm for 60 minutes, the temperature is at 50~52 ℃, then cool down, the temperature is down to 25 ℃, spent 60 minutes. Crystallization is over. The crystallization liquid is extracted in vacuum, washed with 120ml of acetone, drained, the tetracycline hydrochloride wet product after the extraction is put into an oven for drying, and taken out after 30 minutes to obtain tetracycline hydrochloride 67g, measure its moisture content 0.33%.

Embodiment 2

[0017] Weigh 200g of tetracycline wet alkali with a water content of 15%. According to the ratio of tetracycline (dried): butanol = 1:5-6, measure 850ml of butanol at a temperature of 17.5°C. Mix and stir evenly, adjust with 58ml of concentrated hydrochloric acid, measure the solution with pH test paper in the range of pH=1.7~1.9, the solution is clear, and measure its potency unit to be 162546u / ml. Begin to heat up, with 35 minutes solution temperature is raised to 50 ℃, continue to keep warm for 60 minutes, temperature is at 50~52 ℃, then cool down, temperature is down to 25 ℃, spent 60 minutes. Crystallization is over. The crystallization liquid is extracted in vacuum, washed with 240ml of acetone, drained, the tetracycline hydrochloride wet product after the extraction is put into an oven for drying, and taken out after 30 minutes to obtain tetracycline hydrochloride 131g, measure its moisture content 0.24%.

Embodiment 3

[0019] Weigh 1000 g of tetracycline wet alkali with a water content of 15%. According to the ratio of tetracycline (dried): butanol = 1:5-6, measure 4250ml of butanol at a temperature of 19°C. Mix and stir evenly, adjust with 290ml of concentrated hydrochloric acid, measure the solution with pH test paper in the scope of pH=1.7~1.9, the solution is clear, measure its potency unit to be 1491051u / ml. Begin to heat up, with 30 minutes the solution temperature is raised to 51 ℃, continue to keep warm for 60 minutes, the temperature is at 50~52 ℃, then cool down, the temperature is down to 25 ℃, spent 60 minutes. Crystallization is over. The crystallization liquid is extracted in vacuum, washed with acetone of 1200ml, drained, the tetracycline hydrochloride wet product after the extraction is put into an oven for drying, takes out after 30 minutes, weighs tetracycline hydrochloride 663g, measures its moisture content 0.41%.

[0020]

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Abstract

The invention relates to a preparation method of tetracycline hydrochloride. The method firstly mixes tetracycline and butanol evenly, adjusts the pH to 1.7-1.9, then slowly raises the temperature to 50-52°C, heats it for 60-90 minutes, cools down and crystallizes. Vacuum extract the crystallization solution, wash with acetone, drain and dry to obtain tetracycline hydrochloride. The present invention adopts tetracycline to generate tetracycline hydrochloride in one step. Because there is no urea double salt post, the yield loss of one post is reduced. At the same time, because one process is missing, personnel are reduced, production equipment is reduced, urea consumption does not exist, and the production cost of the product is reduced. The advantage of shortening the production process is also reflected in the timely processing of intermediate materials, which greatly shortens the storage and processing time of intermediate materials, effectively reduces the probability of tetracycline degradation reactions, and improves product quality.

Description

technical field [0001] The present invention relates to biological and new medical technology, in particular to a preparation method of tetracycline hydrochloride. Background technique [0002] In the prior art, the production method of tetracycline hydrochloride is: first react tetracycline and urea to generate urea double salt, then dissolve the urea double salt in butanol, and crystallize to generate tetracycline hydrochloride. In the process of converting tetracycline into urea tetracycline, the method has yield loss, urea consumption, and staff wages, resulting in increased production cost of the product. Contents of the invention [0003] The object of the present invention is to overcome the defective of above-mentioned prior art, provide a kind of effectively improve product yield, reduce labor intensity, reduce production equipment and personnel, improve the preparation method of the tetracycline hydrochloride of the clarithromycin of working production environmen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/12C07C231/24
Inventor 沈伟军马晓军罗江涛李学兵张志
Owner NINGXIA QIYUAN PHARMA
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