Preparation method of doxycycline monohydrate

A technology for doxycycline and doxycycline hydrochloride, which is applied in the field of compound preparation, can solve the problems of complex process, low yield, toxic sulfosalicylic acid, etc., and achieves stable material quality, high raw material yield and high technological simple effect

Active Publication Date: 2021-08-17
ZHENJIANG GAOHAI BIOLOGICAL PHARMA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] "A method for producing doxycycline monohydrate (CN106946728A)" discloses a preparation method of doxycycline monohydrate, but the method is complex (after obtaining the doxycycline monohydrate crude product In the purification process, sulfosalicylic acid is used to precipitate salt-forming substances, and sulfosalicylic acid is toxic, difficult to degrade, and difficult to recycle. If it is directly discharged or handled improperly, it will pollute the environment and cause harm to the human body)

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  • Preparation method of doxycycline monohydrate

Examples

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Example Embodiment

[0033] Example 1

[0034] The preparation method of Danyi Cerporate aid is as follows:

[0035] (1) 70% ethanol 1250 kg in 20001, the yellow hydrochloride is 500kg, and the end of the hydrochloride, the end is lowered to 0 ° C, and the increase of ammonia water is slowly added to 200KG, and the temperature is not More than 10 ° C. The treatment is gradually changed from yellow, and the pH is continuously tested (once every 3 minutes), control pH ≤ 7.5, stirred to complete dissolution, and stirring for 10 minutes.

[0036] (2) After confirming that the pH is not changed, slowly add the high pre-filtered CP hydrochloric acid, adjust the pH to 6.00 at one time, heat the solution to heat the solution to 50 ° C, heat insulation half an hour, precipitate Double West Cerclone A hydrocrystal crystal, the cooling water is stirred for 1.5 hours, and the crystals are precipitated. The filter cake is filtered with centrifuge, and the filter cake is rinsed with a deionized water 30 kg and 50 k...

Example Embodiment

[0037] Example 2

[0038] The preparation method of Danyi Cerporate aid is as follows:

[0039] (1) 70% ethanol 1000 kg in 20001, the yellow hydrochloride is 500kg, and the end of the hydrochloride is 500kg, and the end is lowered to -5 ° C, and the ammonia water is slowly added dropwise to 150kg, maintain the temperature of the solution. No more than 10 ° C. The treatment is gradually changed from yellow, and the pH is continuously tested with precision test strips (once every 4 minutes), control pH ≤ 7.5, stirred until allorate, continued to stir for 7 minutes.

[0040] (2) After confirming that the pH does not change, slowly add the high pre-filtered CP hydrochloric acid, adjust the pH to 6.50 in one time, heat the solution to heat the solution to 45 ° C, heat insulation for half an hour, precipitate Double West Cerclone One aquifer crystal, the cooling water is stirred for 1.5 hours, all precipitated crystals, filter with centrifuge, filter cake, 30 kg of ethanol and 50 kg of ...

Example Embodiment

[0041] Example 3

[0042] (1) 70% ethanol 1,500 kg was put into 20001, and the yellow hydrochloride was put into yellow hydrochloride. The end of the mixture was lowered to 10 ° C, and the high level of ammonia was slowly added dropwater by 250 kg, and the temperature of the solution was not allowed. More than 15 ° C. The treatment is gradually changed from yellow, and the pH is continuously tested with a precise test strip (once every 5 minutes), control pH ≤ 7.5, stirred until the whole dissolved, and stirring for 5 minutes.

[0043] (2) After confirming that the pH does not change, slowly add the high pre-filtered CP hydrochloric acid, adjust the pH to 5.50 at one time, heat the solution to heat the solution to 38 ° C, heat insulation half an hour, precipitate Double-west One aquatic crystal, the cooling water is stirred down for 2 hours, all precipitated crystals, filter with centrifuge, filter cake, 30 kg and ethanol, 50 kg, sufficiently dried (at 80-95 ° C) Hot water heating...

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Abstract

The invention discloses a preparation method of a doxycycline monohydrate. The method comprises the following steps: (1) adding doxycycline hydrochloride into ethanol, cooling the obtained solution, then dropwise adding ammonia water into the solution, keeping the temperature of the solution not more than 15 DEG C and the pH value of the solution not more than 7.5, and stirring until the doxycycline hydrochloride is completely dissolved; and (2) adjusting the pH value of the solution obtained in the previous step to 5.50-6.50 by using acid, then separating out doxycycline monohydrate crystals by using a crystallization method, filtering, washing and drying. The doxycycline monohydrate which is stable in quality, high in purity and low in impurity content is prepared through the method, the process is simple and environmentally friendly, the raw material yield is high, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation method of doxycycline monohydrate. Background technique [0002] Doxycycline monohydrate is a broad-spectrum bacteriostatic agent with bactericidal effect at high concentrations. Many rickettsia, mycoplasma, chlamydia, atypical mycobacteria, and spirochetes are also sensitive to this product. This product has a better effect on Gram-positive bacteria than Gram-negative bacteria, but Enterococcus is resistant to it. Others such as Actinomycetes, Bacillus anthracis, Listeria monocytogenes, Clostridium, Nocardia, Vibrio, Brucella, Campylobacter, and Yersinia are sensitive to this product. [0003] The fat solubility of doxycycline monohydrate is 5 times larger than that of tetracycline and 50 times larger than that of oxytetracycline. Its antibacterial spectrum is the same as that of tetracycline, but its effect is 2 to 10 times stronger than...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/12C07C231/24
CPCC07C231/12C07C231/24C07C2603/46C07C237/26Y02A50/30
Inventor 李义高庄旭祥李小彪赵阳
Owner ZHENJIANG GAOHAI BIOLOGICAL PHARMA CO LTD
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