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A kind of preparation method of doxycycline hydrochloride and the doxycycline hydrochloride prepared by this method

A technology of doxycycline hydrochloride and oxytetracycline, which is applied in the preparation of sulfonate, carboxylic acid amide, and organic compound, which can solve the problems of unrecyclable solvents and unstable yields, and reduce environmental pollution. Effects of pollution and waste of resources, stable product yield, and reduction of by-products

Active Publication Date: 2021-04-16
河南后羿制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is the problem that the yield is unstable and the solvent in the preparation process cannot be recycled

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of doxycycline hydrochloride, comprising the following steps:

[0022] (1) Preparation of chlorinated antipyretic ice

[0023] In a 3 L glass-lined reaction tank, put 0.82 L of drinking water, add 150 g of baking soda, adjust the pH to 8-9, start stirring for about 30 minutes, then put in 231 g of antipyretic ice, open the interlayer to freeze and cool down to 10-15 ℃. Slowly add metered sodium hypochlorite along the tank wall, control the temperature not to exceed 15°C, stir for 60 minutes after the addition is complete, and discharge and shake off the filter after the end point is reached. The filter cake was washed to pH 7 with potable water. Fully dry the filter cake for 1 hour to obtain chlorinated antipyretic ice, and put it in a cold storage for later use.

[0024] (2) Oxytetracycline chloride—11-α-chloro-6,12-hemiketal Oxytetracycline

[0025] Add 0.45 L of methanol into a 1L glass-lined reaction tank, add 50 g of oxytetracycline base un...

Embodiment 2

[0036] A preparation method of doxycycline hydrochloride, comprising the following steps:

[0037] (1) Preparation of chlorinated antipyretic ice

[0038] In a 3 L glass-lined reaction tank, put 0.81 L of drinking water, add 151 g of baking soda, adjust the pH to 8-9, start stirring for about 30 minutes, then put in 231 g of antipyretic ice, open the interlayer to freeze and cool down to 10-15 ℃. Slowly add metered sodium hypochlorite along the tank wall, control the temperature not to exceed 15°C, stir for 60 minutes after the addition is complete, and discharge and shake off the filter after the end point is reached. The filter cake was washed to pH 7 with potable water. Fully dry the filter cake for 1 hour to obtain chlorinated antipyretic ice, and put it in a cold storage for later use.

[0039] (2) Oxytetracycline chloride—11-α-chloro-6,12-hemiketal Oxytetracycline

[0040] Add 0.46 L of methanol into a 1L glass-lined reaction tank, add 50.2 g of oxytetracycline base ...

Embodiment 3

[0051] A preparation method of doxycycline hydrochloride, comprising the following steps:

[0052] (1) Preparation of chlorinated antipyretic ice

[0053] In a 3 L glass-lined reaction tank, put 0.79 L of drinking water, add 150 g of baking soda, start stirring for about 30 minutes, then put in 231 g of antipyretic ice, open the interlayer to freeze and cool down to 10-15 °C. Slowly add metered sodium hypochlorite along the tank wall, control the temperature not to exceed 15°C, stir for 60 minutes after the addition is complete, and discharge and shake off the filter after the end point is reached. The filter cake was washed to pH 7 with potable water. Fully dry the filter cake for 1 hour to obtain chlorinated antipyretic ice, and put it in a cold storage for later use.

[0054] (2) Oxytetracycline chloride—11-α-chloro-6,12-hemiketal Oxytetracycline

[0055] Add 0.45 L of methanol into a 1L glass-lined reaction tank, add 49.9 g of oxytetracycline base under stirring, slowly...

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PUM

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Abstract

The present invention provides a kind of preparation method of doxycycline hydrochloride and the doxycycline hydrochloride prepared by this method, provide raw material through the reaction of chlorinated antipyretic ice and oxytetracycline, improve the productive rate of doxycycline hydrochloride, The generation of by-products is reduced, and the antipyretic ice, ethanol, methanol, etc. in the preparation process can be recycled, environmental pollution and resource waste are reduced, and the production cost is reduced, and the product yield in the preparation process of the method is stable. In addition, the doxycycline hydrochloride prepared by the preparation method of the present invention has high purity and good color.

Description

technical field [0001] The invention relates to a preparation method of doxycycline hydrochloride and doxycycline hydrochloride prepared by the preparation method. Background technique [0002] Doxycycline hydrochloride is a broad-spectrum semi-synthetic tetracycline antibiotic, mainly used for upper respiratory tract infection, tonsillitis, biliary tract infection, lymphadenitis, cellulitis, etc. caused by sensitive gram-positive bacteria and gram-negative bacilli , It is also used to treat typhus, Qiang insect disease, mycoplasma pneumonia, etc. It can also be used to treat cholera, and can also be used to prevent falciparum malaria and leptospira infection. The medicine has strong water solubility, good absorption and wide distribution, and has many clinical applications and good effects. Clinical veterinary medicine is mainly used for the treatment of livestock and poultry respiratory diseases, Escherichia coli, Salmonella, etc. [0003] Doxycycline hydrochloride is st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/12C07C237/26
CPCC07C231/12C07C303/32C07C237/26C07C309/04C07C309/60
Inventor 王凯李建正李星万毅尚鹤华李盼
Owner 河南后羿制药有限公司
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