Preparation method of chlorinated oxytetracycline

A technology of oxytetracycline chloride and formula, applied in the field of preparation of oxytetracycline chloride, can solve the problems of high risk, high processing cost, explosion, etc., and achieve simple operation and post-processing, economical and environmentally friendly process, and economical process Another effect

Active Publication Date: 2020-07-10
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) Although the reactant N-chlorosuccinimide is used in less amount and has low toxic and side effects, it is a corrosive substance, and its toxic and side effects are still harmful to the human body. Larger, inhalation or sticking to the skin can cause burns, serious cases even need to be sent to the hospital for diagnosis and treatment, and the environment is harmful;
[0007](2) The filtered waste liquid contains excessive N-chlorosuccinimide, and the treatment cost is relatively high;
[0008](3) N-chlorosuccinimide is sensitive to moisture and has poor stability; the preparation process of the chlorinating agent itself is complicated and risky. There is a risk of explosion when the chlorination reaction temperature is higher than 8°C during the process

Method used

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  • Preparation method of chlorinated oxytetracycline
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  • Preparation method of chlorinated oxytetracycline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A preparation method of oxytetracycline, comprising the following steps:

[0033] (1) Add 350g of purified water into a 500ml four-necked bottle equipped with a thermometer and mechanical stirring, heat up to 55-60°C, add 12.9g of pulverized cyanuric acid at one time and stir to completely dissolve;

[0034] (2) Slowly feed chlorine into the cyanuric acid solution obtained in step (1) four-necked bottle, the chlorine quality is controlled at 6.8~7.1g, and the solution pH value is controlled between 2.0~2.5 for 1.5h;

[0035] (3) After the reaction is completed, heat-filter the solid-liquid mixture obtained in step (2), rinse the filter cake with 20 g of 55-60°C hot water for 1-2 times, and dry it in an oven at 70-80°C to obtain monochlorine 13.54g of isocyanuric acid solid is used for later use. After testing, the solid liquid phase content of monochloroisocyanuric acid is 96.45%, and the molar yield is 79.85%;

[0036] (4) Add 300g methanol to another 500ml four-neck...

Embodiment 2

[0040] A preparation method of oxytetracycline, comprising the following steps:

[0041] (1) Add 350g of purified water into a 500ml four-necked bottle equipped with a thermometer and mechanical stirring, heat up to 55-60°C, add 12.9g of pulverized cyanuric acid at one time and stir to completely dissolve;

[0042] (2) Slowly feed chlorine into the cyanuric acid solution obtained in step (1) four-necked bottle, the quality of chlorine is controlled at 6.8~7.1g, and the pH value of the solution is controlled between 2.5~3.0 for 1.5h;

[0043] (3) After the reaction is completed, heat-filter the solid-liquid mixture obtained in step (2), rinse the filter cake with 20 g of 55-60°C hot water for 1-2 times, and dry it in an oven at 70-80°C to obtain monochlorine 15.83g of isocyanuric acid solid is used for later use. After testing, the solid-liquid phase content of monochloroisocyanuric acid is 98.30%, and the molar yield is 95.51%;

[0044] (4) Add 300g methanol to another 500ml...

Embodiment 3

[0048] A preparation method of oxytetracycline, comprising the following steps:

[0049] (1) Add 350g of purified water into a 500ml four-necked bottle equipped with a thermometer and mechanical stirring, heat up to 55-60°C, add 12.9g of pulverized cyanuric acid at one time and stir to completely dissolve;

[0050] (2) Slowly feed chlorine into the cyanuric acid solution obtained in step (1) four-necked bottle, the chlorine quality is controlled at 6.8~7.1g, and the solution pH value is controlled between 3.0~3.5 for 1.5h;

[0051] (3) After the reaction is completed, heat-filter the solid-liquid mixture obtained in step (2), rinse the filter cake with 20 g of 55-60°C hot water for 1-2 times, and dry it in an oven at 70-80°C to obtain monochlorine 14.39g of isocyanuric acid solid is used for later use. After testing, the solid liquid phase content of monochloroisocyanuric acid is 97.28%, and the molar yield is 85.60%;

[0052](4) Add 300g methanol to another 500ml four-necke...

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PUM

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Abstract

The invention relates to a preparation method of chlorinated oxytetracycline. The preparation method can be widely applied to the technical field of veterinary drugs and solves the technical problemsof large toxic and side effects, large environmental harm, high waste liquid treatment cost and poor intermediate product stability in the existing preparation method of chlorinated oxytetracycline. The reaction equations are as follows: a first-step chemical reaction equation; and a second-step chemical reaction equation.

Description

technical field [0001] The invention relates to the technical field of veterinary medicine, in particular to a preparation method of oxytetracycline chloride. Background technique [0002] The full name of oxytetracycline chloride is 11α-chloro-6,12 hemiketal oxytetracycline, and its structural formula is as follows: [0003] [0004] Oxytetracycline chloride is an important intermediate product in the production of doxycycline (doxycycline hydrochloride), which is obtained from oxytetracycline through a chlorination reaction and used to prepare 11α-chloro-6-methine oxytetracycline , and 11α-chloro-6-methine oxytetracycline is an important intermediate for the production of doxycycline. Doxycycline is a kind of antibiotic. In addition, the drug is also widely used in veterinary medicine. It has antibacterial effect on various cocci and bacillus, and has inhibitory effect on Rickettsia and Plasmodium amoeba. For the treatment of respiratory infections, urinary tract infe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/26C07C231/12
CPCC07D251/36C07C231/12C07C237/26Y02A50/30
Inventor 张建强李琦斌刘聪郭兴龙达先鹏
Owner SHANDONG GUOBANG PHARMA
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