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Method for preparing high-purity tetracycline hydrochloride

A technology of tetracycline hydrochloride and tetracycline, which is applied in the preparation of carboxylic acid amide, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of poor quality of crystallized products, achieve quality improvement, optimize temperature control process, and no coalescence Effect

Active Publication Date: 2015-03-04
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the deficiencies of existing methods and the poor quality of crystallized products, the invention discloses a method for preparing tetracycline hydrochloride with a purity of more than 98%.

Method used

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  • Method for preparing high-purity tetracycline hydrochloride
  • Method for preparing high-purity tetracycline hydrochloride
  • Method for preparing high-purity tetracycline hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 30g of tetracycline urea double salt (0.0624 mol) in 150ml of n-butanol and 100ml of methanol mixed solvent, stir at 10°C for 5 minutes, add 6.1ml of concentrated hydrochloric acid (HCl 0.0626 mol) with a mass concentration of 37.5%, and continue stirring After filtering. Move the filtrate into the crystallizer, add 1.0g of seed crystals at a heating rate of 2°C / min to 30°C, continue to maintain the same heating rate until 40°C, maintain constant temperature for 30 minutes, and then cool down at a rate of 3°C / min The rate was reduced to 20 °C. The crystalline product is filtered, washed with acetone, and dried at 40°C for 12 hours under a vacuum of 0.05 MPa. The final crystalline product has a purity of 98.3% and a main particle size of 210 μm. The product quality meets the standards of the Chinese Pharmacopoeia 2000 edition. The scanning electron micrographs of the crystalline products are as follows figure 1 As shown, the product particle size distribution ...

Embodiment 2

[0026] Dissolve 30g of tetracycline urea double salt (0.0624 mol) in 270ml of n-butanol and 30ml of methanol mixed solvent, stir at 15°C for 5 minutes, add 12.3ml of 30% concentrated hydrochloric acid (HCl 0.101 mol), and continue stirring After filtering. Move the filtrate into the crystallizer, add 0.3g of seed crystals at a heating rate of 8°C / min to 32°C, continue to maintain the same heating rate until 50°C, maintain constant temperature for 20 minutes, and then cool down at a rate of 5°C / min The rate was reduced to 15 °C. The crystalline product is filtered, washed with acetone, and dried for 4 hours at 45°C under a vacuum of 0.1 MPa. The purity of the final crystalline product is 98.1%, and the main particle size is 205 μm. The product quality meets the standards of the Chinese Pharmacopoeia 2000 edition.

Embodiment 3

[0028] Dissolve 30g of tetracycline urea double salt (0.0624 mol) in 150ml of n-butanol and 60ml of ethanol mixed solvent, stir at 15°C for 8 minutes, add 7.3ml of concentrated hydrochloric acid (HCl 0.072 mol) with a mass concentration of 36%, and continue stirring filter. Move the filtrate into the crystallizer, add 0.6g of seed crystals at a heating rate of 1°C / min to 27°C, continue to maintain the same heating rate until 48°C, maintain constant temperature for 40 minutes, and then cool down at a rate of 4°C / min The rate was reduced to 10 °C. The crystalline product is filtered, washed with acetone, and dried at 50°C for 8 hours under a vacuum of 0.06 MPa. The final crystalline product has a purity of 98.2% and a main particle size of 220 μm. The product quality meets the standards of the Chinese Pharmacopoeia 2000 edition.

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Abstract

The invention relates to a method for preparing high-purity tetracycline hydrochloride. Tetracycline urea double salt and hydrochloric acid serve as raw materials, and reaction of the tetracycline urea double salt and hydrochloric acid and crystallization of tetracycline hydrochloride are simultaneously performed. The method comprises the following steps of: mixing the double salt with an organic alcohol mixed solvent according to a ratio, adding hydrochloric acid at the temperature of 5-20 DEG C, continuously stirring and filtering; transferring the filtrate into a crystallizer, raising the temperature, adding a seed crystal when the system temperature reaches 27-32 DEG C, further raising the temperature to 40-50 DEG C, and growing the grain at constant temperature; reducing the temperature of the suspension to 5-20 DEG C; and filtering, washing and drying the obtained crystal mush, thereby obtaining a tetracycline hydrochloride crystal product. The reaction and crystallization processes in the solvent system are screened and optimized, the tetracycline hydrochloride crystal which is uniform in particle size distribution, zero in coalescence and complete in crystalline form and has the purity of more than 98.0 percent is obtained, and the process yield is more than 88.0 percent. The problems that the product is non-uniform in particle size distribution and severe in coalescence so that the purity of the product is reduced are solved, and the product quality is obviously improved.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, and in particular relates to a method for preparing tetracycline hydrochloride by reacting and crystallizing tetracycline urea double salt and hydrochloric acid as raw materials. Background technique [0002] The chemical name of Tetracycline Hydrochloride is 2-Naphthacenecarboxamide,4-(dimethylamino)-1,4,4a,5,5a,6,11,12a-octahydro-3,6,10,12,12a-pentahydro- 6-methyl-1,11-dioxo-, monohydrochloride, (4S, 4aS, 5aS, 6S, 12aS) (CAS: 64-75-5), molecular formula C 22 h 24 N 2 o 8 HCl, the molecular weight is 480.90, its chemical structure is as follows: [0003] [0004] Tetracycline hydrochloride is the first generation of tetracycline antibiotics. It has broad-spectrum antibacterial properties and can resist various microorganisms such as Gram-negative and Gram-positive bacteria, Chlamydia, Mycoplasma, Rickettsia and protozoan parasites. . In addition, for many pe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/12
Inventor 郝红勋王永莉尹秋响侯宝红赵琰张美景谢闯王静康鲍颖
Owner TIANJIN UNIV
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