Method for preparing cefmenoxime hydrochloride compound

摘要

A novel process for purifying Cefmenoxime hydrochloride comprises: 1) adding a solvent wherein Cefmenoxime hydrochloride is insoluble at the temperature less than 30° C., filtering after vigorous stirring, washing the filter cake with a solvent wherein Cefmenoxime hydrochloride is insoluble at a temperature less 20° C., and drying; 2) placing the filter cake into ammonium hydroxide, controlling the pH value less than 9 with a gentle agitation to obtain Cefmenoxime acid solution in ammonium hydroxide, and then filtering out the precipitate; 3) adding hydrochloric acid at a concentration of 0.5-4 mol/L to Cefmenoxime acid solution in ammonium hydroxide slowly and controlling the temperature between 30-60° C. and the final pH between 0.5-3.0, and then cooling down to a minimum of 10° C. and standing still to allow crystallization, filtrating and vacuum drying.

主权项

1. A novel process for purifying Cefmenoxime hydrochloride of the following formula, characterized in that the process comprises: step 1) adding a solvent wherein Cefmenoxime hydrochloride is insoluble to the raw Cefmenoxime hydrochloride while controlling the temperature at the range between 10 and 30° C., filtering after vigorous stirring, washing the filter cake with a solvent wherein Cefmenoxime hydrochloride is insoluble at a temperature between 0 and 20° C., and drying in vacuum or in the air; step 2) placing the filter cake into ammonium hydroxide, controlling the pH value between 7 and 9 with a gentle agitation to obtain Cefmenoxime acid solution in ammonium hydroxide, and then filtering out the precipitate; step 3) adding hydrochloric acid at a concentration of 0.5-4 mol/L to the Cefmenoxime acid solution in ammonium hydroxide and controlling the temperature between 30° C. and 60° C., and the final pH between 0.5 and 3.0 in 30 minutes to 5 hours, and then cooling down to 10° C. and standing still to allow crystallization, filtrating and vacuum drying to obtain the refined Cefmenoxime hydrochloride; and step 4) optionally, recycling the remaining liquid of step 3) for the recrystallization in step 3).