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Production method of chlortetracycline bisulfate

A technology of bisulfate and production method, applied in the separation/purification of carboxylic acid amide, organic chemistry and other directions, can solve the problems of increasing solvent recovery cost, reducing product competitiveness, increasing manufacturing cost, etc., to shorten production cycle and improve safety Productivity, the effect of reducing production costs

Active Publication Date: 2014-04-23
FUJIAN FUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using 2-ethoxyethanol to dissolve, adding n-butanol or methanol to crystallize the dissolution and crystallization method, on the one hand, the mother liquor contains two kinds of solvents, which leads to increased solvent recovery costs, thereby increasing manufacturing costs and reducing product competitiveness; On the one hand, because alcohol will combine with aureomycin hydrogen sulfate to generate aureomycin hydrogen sulfate solvate, the product will contain 2-ethoxyethanol (≤18%) and n-butanol (≤15%) or methanol (≤ 7%) solvent residues, affecting product quality

Method used

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  • Production method of chlortetracycline bisulfate
  • Production method of chlortetracycline bisulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Add 8kg of ethanol to the preparation tank, add 2kg of sulfuric acid dropwise under the temperature of 40°C, after dropping, stir for 10min, and store it at room temperature for later use; After the ethanol mixture is added dropwise, control the temperature at 20°C and stir for 30 minutes, then filter; after filtering, collect the filtrate in a crystallization tank, control the temperature at 35°C and then add 16kg of ethanol dropwise, after the dropwise addition of ethanol, keep it warm for 3 hours, and slowly cool down to 10 Insulate at ℃ for 2 hours; filter to obtain the filter cake, wash the filter cake with 32kg of ethanol, and then filter to obtain the wet powder; dry the wet powder in vacuum, control the temperature at 40°C, and dry at a vacuum degree of -0.07~-0.10Mpa until the weight loss on drying is ≤2.0%. Get aureomycin bisulfate 11.5kg, and the weight yield is 115%. The quality of the product complies with the standards of the United States Pharmacopoeia; a...

Embodiment 2

[0026] Add 12kg of ethanol to the preparation tank, and add 3kg of sulfuric acid dropwise under the control temperature of 40°C. After the dripping is completed, stir for 15min, and store it for later use at normal temperature; After the ethanol mixture is added dropwise, control the temperature at 25°C and stir for 30 minutes, then filter; after filtering, collect the filtrate in a crystallization tank, control the temperature at 40°C and then add 20kg of ethanol dropwise, after the dropwise addition of ethanol, keep it warm for 3 hours, and slowly cool down to 12 Insulate at ℃ for 2 hours; filter to obtain the filter cake, wash the filter cake with 40kg of ethanol, and then filter to obtain the wet powder; vacuum-dry the wet powder at a controlled temperature of 45°C and a vacuum degree of -0.07~-0.10Mpa until the drying weight loss ≤ 2.0%, to obtain Chlortetracycline hydrogen sulfate 11.2kg, weight yield is 112%. The quality of the product complies with the standards of the...

Embodiment 3

[0028] Add 16kg of ethanol to the preparation tank, add 4kg of sulfuric acid dropwise under the control temperature of 40°C, after dropping, stir for 20min, store it at room temperature for later use; After the ethanol mixture is added dropwise, control the temperature at 30°C and stir for 30 minutes, then filter; after filtering, collect the filtrate in a crystallization tank, control the temperature at 45°C and then add 24 kg of ethanol dropwise, after the dropwise addition of ethanol, keep warm for 3 hours, and slowly cool down to 15 Insulate at ℃ for 2 hours; filter to obtain the filter cake, wash the filter cake with 48kg of ethanol, and then filter to obtain wet powder; vacuum dry the wet powder at a controlled temperature of 50°C and vacuum degree of -0.07~-0.10Mpa until the drying weight loss ≤ 2.0%, Get aureomycin bisulfate 11.1kg, and the weight yield is 111%. The quality of the product complies with the standards of the United States Pharmacopoeia; after being store...

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Abstract

The invention discloses a production method of chlortetracycline bisulfate. The production method comprises the following steps: dropping a well prepared sulfuric acid / ethanol mixed solution in an ethanol suspension of a chlortetracycline base to dissolve the chlortetracycline base, filtering, then performing crystal growth by using ethanol, filtering, further washing with the ethanol, filtering, and finally performing vacuum drying to obtain the chlortetracycline bisulfate. According to the preparation method disclosed by the invention, the operation procedure is simplified, the production period is shortened, a single solvent is used to facilitate the recovery and the mechanical application of the solvent, the production cost is reduced, and the safety in production, the yield and the product quality are further improved. The chlortetracycline bisulfate prepared by the preparation method disclosed by the invention has the advantages of high yield, high titer, low solvent residue and good stability.

Description

technical field [0001] The invention relates to a production method of aureomycin hydrogen sulfate. Background technique [0002] Aureomycin is the active ingredient in the biosynthesis of Streptomyces aureofaciens, and it is a tetracycline antibiotic. Chlortetracycline hydrochloride is the hydrochloride salt of aureomycin. As a human medicine, it is mainly used to treat conjunctivitis and trachoma. As a veterinary medicine, it is mainly used to treat diseases such as typhoid fever and pullorum in livestock. It can also be used as a growth promoter for livestock. In recent years, with the further development of animal husbandry, the market demand for aureomycin hydrochloride has been continuously expanding. [0003] Compared with Chlortetracycline Hydrochloride, Chlortetracycline Bisulfate has very good water solubility and thus has higher medicinal value. The water mixture of chlortetracycline bisulfate is very clear and does not contain small particles that can block the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/26C07C231/24
Inventor 张发香
Owner FUJIAN FUKANG PHARMA
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