参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | Carbonic acid sodium salt (1:2) | HCID 10340 | — |
| 反应物 | 碳酸钾 | HCID 11430 | — |
| 反应物 | 红霉素 | HCID 12560 | — |
| 反应物 | 硫氰酸红霉素 | HCID 83938 | — |
| 反应物 | 碳酸氢钠 | HCID 516892 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 溶剂 | 乙醚 | HCID 3283 | — |
| 产物 | 琥乙红霉素 | HCID 443953 | — |
反应步骤
or method B: 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 one or more of erythromycin thiocyanate or erythromycin thiocyanate hydrate, erythromycin lactate, stirred, added sodium bicarbonate or sodium carbonate or potassium carbonate, and water, allowed to react with stirring for 1-3 hours, added dropwise an aqueous solution of an acid or a base, stirred to control the pH value at about 7.0-8.5; the organic phase is precipitated and separated; to the organic phase is added sodium bicarbonate or sodium carbonate or potassium carbonate, and water, stirred, cooled to 20° C. or below, added monoethyl succinate halide, including monoethyl succinate chloride or monoethyl succinate bromide, allowed to react, 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.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 专利号 | US09221862B2 |
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| 来源数据集 | uspto-grants-2015_12 |
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| ORD ID | ord-e3150fef325d4fa8aa271398501c6ae5 |
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| 来源说明 | uspto-grants-2015_12 |
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