Preparation method of large-grain occrycetin

A technology of oxytetracycline hydrochloride and large particles is applied in the field of preparation of large particles of oxytetracycline hydrochloride, which can solve the problems of high consumption of oxytetracycline and butanol, difficult recovery of butanol, influence on performance of use, and the like, and achieves easy recovery , the effect of low cost and short crystallization time

Active Publication Date: 2010-09-08
CHIFENG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are reports in the literature; the mixture of butanol, butanol and other lower fatty alcohols or lower fatty esters of acetic acid is used as a solvent, reacted with hydrochloric acid, crystallized, separated, and dried to obtain large particle ox

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: the preparation method of large particle oxytetracycline hydrochloride, comprises the following steps: (1) in 50L purified water, add reagent hydrochloric acid 10L, stir and add 50kg oxytetracycline, after dissolving completely, add 10L methyl alcohol, stir, Filter through a plate and frame to obtain the filtrate; (2) Stir and add 6L saturated potassium chloride solution, 2L reagent hydrochloric acid and 0.5kg seed crystal to the filtrate, stand for crystallization at 20-22°C for 1 hour, centrifuge, and filter cake Wash with 50L of anhydrous methanol to obtain a wet product; (3) the wet product is dried by a vacuum drier at a temperature of 92 to 98° C. and a vacuum of 0.08 MPa for 8 hours to obtain 40.1 kg of a large particle oxytetracycline hydrochloride finished product.

Embodiment 2

[0013] Embodiment 2: the preparation method of large particle oxytetracycline hydrochloride comprises the following steps; (1) add reagent hydrochloric acid 9L in 70L purified water, stir and add 50kg oxytetracycline, after dissolving completely, add 40L methyl alcohol, stir, Filter through a plate and frame to obtain the filtrate; (2) Stir and add 4L saturated ammonium chloride solution, 8L reagent hydrochloric acid and 0.5kg seed crystal to the filtrate, stand for crystallization at 20-22°C for 1 hour, centrifuge, and filter cake Wash with 50L of anhydrous methanol to obtain a wet product; (3) the wet product is dried by a vacuum drier at a temperature of 92 to 98° C. and a vacuum of 0.08 MPa for 8 hours to obtain 42.2 kg of large particle oxytetracycline hydrochloride finished product.

Embodiment 3

[0014] Embodiment 3: the preparation method of large particle oxytetracycline hydrochloride comprises the following steps; (1) add reagent hydrochloric acid 12L in 85L purified water, stir and add 50kg oxytetracycline, after dissolving completely, add 70L methyl alcohol, stir, Filter through a plate and frame to obtain the filtrate; (2) Stir and add 7L hydrochloric acid and 0.5kg seed crystals to the filtrate, stand for crystallization at a temperature of 19-22°C for 1 hour, centrifuge, and wash the filter cake with 50L anhydrous methanol to obtain Wet product; (3) wet product is dried by vacuum drier, temperature 92~98 ℃, vacuum tightness 0.08MPa, dry 8 hours, get large particle oxytetracycline hydrochloride finished product 40.5kg.

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PUM

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Abstract

The invention discloses a preparation method of large-grain occrycetin, comprising the following steps of: adding hydrochloric acid to purified water; adding terramycin under stirring; adding methanol after compete dissolution, uniformly stirring, and filtering to obtain filter liquor; adding a high-concentration aqueous salt solution containing chloridions to the filter liquor under stirring, and also adding the hydrochloric acid and a small quantity of seed crystals; standing, and crystallizing to separate out an occrycetin crystallized wet product; and drying through a vacuum dryer to obtain the large-grain occrycetin. In the invention, an aqueous methanol solution is used as a solvent because the methanol not only has low price but also is easy to recover, the harm on personnel and anenvironment is reduced because the methanol has little volatilization loss at room temperature, short crystallization time and energy saving are achieved by standing and crystallizing at normal temperature; and the produdct has good flowability, good water solubility and alcohol solubility, high yield coefficient reaching more than 81 percent, terramycin consumption reduction and low cost.

Description

technical field [0001] The invention belongs to the technical field of chemical preparation of compounds, and in particular relates to a preparation method of large particle oxytetracycline hydrochloride. Background technique [0002] Oxytetracycline hydrochloride is a widely used broad-spectrum antibiotic drug; most of the oxytetracycline hydrochloride currently on the market is a fine single crystal powder with poor fluidity, and it is easy to mix with other materials during production and use. Inhomogeneity brings inconvenience to production. Therefore, some users require the use of large particles of oxytetracycline hydrochloride with good fluidity; . The traditional preparation method of oxytetracycline hydrochloride is: dissolve oxytetracycline in the anhydrous methanol solution containing hydrogen chloride (or calcium chloride), through decolorization, filter; add appropriate amount of hydrogen chloride methanol solution in the filtrate, freeze crystallization, centr...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/12C07C231/24
Inventor 鲍国清高峰
Owner CHIFENG PHARMA CO LTD
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