Preparation method of large-grain occrycetin

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...

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 oxytetracycline hydrochloride; however, the yield Low, butanol is not easy to recover, the consumption of oxytetracycline and butanol is high, and the production cost is high; and the product has poor water solubility, which affects the performance of the product