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 | 碳酸氢钠 | HCID 516892 | — |
| 反应物 | Monoethyl succinate chloride | HCID 18404837 | — |
| 反应物 | Monoethyl succinate bromide | HCID 86718268 | — |
| 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
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;
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-75738953660c40d2a5f43ae562378a52 |
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| 来源说明 | uspto-grants-2015_12 |
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