Sodium Carbonate → Erythromycin ethyl succinate

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

The process for preparing erythromycin ethylsuccinate hydrate comprises: method A. in a reaction vessel, one or more of a C1-C6 lower alcohol, a C2-C6 lower nitrile, a C3-C8 lower ketone or C2-C8 lower ether is used as a solvent, to the solvent is added erythromycin, stirred at a temperature of 0-50° C. to dissolve erythromycin; to the solution is added sodium bicarbonate or sodium carbonate or potassium carbonate, and water, stirred, and cooled to 20° C. or below; to the cooled mixture is added monoethyl succinate halide, including monoethyl succinate chloride or monoethyl succinate bromide, allowed to react, and monitored by TLC until the reaction is complete; to the resultant is added an acid or a base to control the pH value at about 7.0-8.5; the organic phase is precipitated and separated; to the organic phase is added water, cooled to −20° C.-10° C.; upon the solid is precipitated completely, the mixture is filtered, the resulting solid is recrystalized with water and one or more of a C1-C6 lower alcohol, a C2-C6 lower nitrile, a C2-C8 lower ether, a C3-C8 lower ketone or C1-C6 lower halogenated hydrocarbons as solvent once or more times, cooled to −20° C.-10° C., filtered, dried to obtain erythromycin ethylsuccinate crystalline hydrate;

Herkunft & Nachweise