反应详情

温度

25 °C

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;

1. stirringstirred
2. temperaturecooled to 20° C. or below
3. customto react
4. additionto the resultant is added an acid
5. customthe organic phase is precipitated
6. customseparated
7. additionto the organic phase is added water
8. temperaturecooled to −20° C.-10° C.
9. customupon the solid is precipitated completely
10. filtrationthe mixture is filtered
11. customthe resulting solid is recrystalized with water and one or more of a C1-C6 lower alcohol
12. temperaturea 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.
13. filtrationfiltered
14. customdried