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 cost, urea consumption, yield loss, etc., and achieves reduction of production equipment and personnel. The effect of reducing and lowering production costs

Active Publication Date: 2016-02-03
NINGXIA QIYUAN PHARMA
View PDF3 Cites 4 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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]

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a preparation method of tetracycline hydrochloride. The preparation method comprises mixing tetracycline and butanol to obtain a uniform mixture, adjusting pH to 1.7-1.9, slowly heating the mixture to a temperature of 50-52 DEG C, carrying out thermal insulation for 60-90min, carrying out cooling crystallization, then carrying out vacuum extraction on the crystallization liquid, carrying out washing by acetone, carrying out vacuum drying and carrying out baking drying to obtain tetracycline hydrochloride. The tetracycline hydrochloride is prepared from tetracycline by one step. A urea double salt process is reduced so that a process yield loss is avoided, workers are reduced, production devices are reduced, a urea loss is avoided and a production cost is reduced. The process flow is shortened so that an intermediate material is timely treated, intermediate material storage and treatment time is greatly shortened, tetracycline degradation reaction probability is effectively reduced and product quality is improved.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap