Preparation method of doxycycline hyclate and doxycycline hyclate prepared through method

A technology of doxycycline hydrochloride and oxytetracycline, which is applied in the preparation of sulfonates, carboxylic acid amides, and organic compounds, etc., can solve the problems such as the inability to recycle the solvent and the unstable yield, and reduce the environmental impact. Pollution and waste of resources, stable product yield, and the effect of reducing the generation of by-products

Active Publication Date: 2019-01-04
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, put in 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 and freeze it to 10-15 °C. Slowly add a metered amount of sodium hypochlorite along the tank wall, and control the temperature not to exceed 15 °C. After adding, stir for 60 minutes. After the end point is reached, discharge and filter. The filter cake was washed to pH 7 with drinking water. The filter cake was fully dried for 1 hour to obtain chlorinated antipyretic ice, which was placed in a cold storage for use.

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

[0025] Add 0.45 L of methanol to a 1 L glass-lined reaction tank, add 50 g of oxytetracycline base under stirring, slo...

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, put in 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 and freeze it to 10-15 °C. Slowly add a metered amount of sodium hypochlorite along the tank wall, and control the temperature not to exceed 15 °C. After adding, stir for 60 minutes. After the end point is reached, discharge and filter. The filter cake was washed to pH 7 with drinking water. The filter cake was fully dried for 1 hour to obtain chlorinated antipyretic ice, which was placed in a cold storage for use.

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

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

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, put in 150 g of baking soda, turn on and stir for about 30 minutes, then put in 231 g of antipyretic ice, and open the interlayer to freeze and cool down to 10-15 °C. Slowly add a metered amount of sodium hypochlorite along the tank wall, and control the temperature not to exceed 15 °C. After adding, stir for 60 minutes. After the end point is reached, discharge and filter. The filter cake was washed to pH 7 with drinking water. The filter cake was fully dried for 1 hour to obtain chlorinated antipyretic ice, which was placed in a cold storage for use.

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

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

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PUM

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Abstract

The invention provides a preparation method of doxycycline hyclate and doxycycline hyclate prepared through the method. Through a reaction between chlorinated acetanilide and oxytetracycline, raw materials are provided. The yield of doxycycline hyclate is increased, production of by-products is reduced, and meanwhile, acetanilide, ethyl alcohol, methyl alcohol and the like generated in a preparation process can be recycled. Therefore, environmental pollution and resource waste are reduced, the production cost is decreased, and the yield of products in the preparation process is stable. Additionally, doxycycline hyclate prepared through the preparation method is high in purity and great in luster.

Description

technical field [0001] The present invention relates to a preparation method of doxycycline hydrochloride and the 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 for the treatment of typhus, qiangiosis, mycoplasma pneumonia, etc. It can still be used for the treatment of cholera, and it can also be used for the prevention of falciparum malaria and leptospirosis infection. The drug has strong water solubility, good absorption and wide distribution, and has many clinical applications and good effects. Clinical veterinary drugs are mainly used for the treatment of respiratory diseases of livestock and poultry, Escherichia coli, Salmonella, etc. ...

Claims

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Application Information

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Patent Type & Authority Applications(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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