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Preparation method of erythromycin ethylsuccinate

A technology of erythromycin ethylsuccinate and erythromycin thiocyanate, applied in the field of medicine, can solve the problems of high cost, high consumption of acid agent and alkali solution, etc., achieves low production cost, reduces the amount of alkali solution, and reduces environmental protection the effect of pressure

Inactive Publication Date: 2017-05-10
HUANGSHI SHIXING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the problem that the amount of acid-binding agent and lye used in the esterification reaction in the preparation process of erythromycin ethylsuccinate in the prior art is large and the cost is high, the purpose of the present invention is to provide a low-cost, environmentally friendly and safe erythromycin ethylsuccinate preparation method

Method used

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  • Preparation method of erythromycin ethylsuccinate
  • Preparation method of erythromycin ethylsuccinate
  • Preparation method of erythromycin ethylsuccinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Preparation of red alkali solution: add 50g erythromycin thiocyanate, 140g tetrahydrofuran, and 77g concentration of 20% potassium carbonate solution (w / w) successively in a three-necked flask, heat up to 40°C, and keep warm for 30min; liquid funnel, let stand for stratification, and separate the water layer; transfer the organic layer into a three-necked flask, add 77g of potassium carbonate solution (w / w) with a concentration of 20%, heat up to 40°C, and keep the temperature for 30min; liquid funnel, let stand to separate the layers, separate the water layer, and obtain the red alkali solution, which will be used in the next esterification reaction.

[0036] Preparation of lye: add 2g of sodium bicarbonate and 20g of sodium carbonate to 28ml of water, stir to obtain lye, set aside.

[0037] Add the above lye into the prepared red alkali solution and stir, lower the temperature to 25°C, add 20g of succinic acid monoethyl chloride dropwise, after the addition is complet...

Embodiment 2

[0039] Preparation of red alkali solution: add 50g erythromycin thiocyanate, 140g tetrahydrofuran, and 77g concentration of 20% potassium carbonate solution (w / w) successively in a three-necked flask, heat up to 40°C, and keep warm for 30min; liquid funnel, let stand for stratification, and separate the water layer; transfer the organic layer into a three-necked flask, add 77g of potassium carbonate solution (w / w) with a concentration of 20%, heat up to 40°C, and keep the temperature for 30min; liquid funnel, let stand to separate the layers, separate the water layer, and obtain the red alkali solution, which will be used in the next esterification reaction.

[0040] Preparation of lye: add 2g of potassium bicarbonate and 20g of potassium carbonate into 28ml of water, stir to obtain lye, set aside.

[0041] Add the above lye into the prepared red alkali solution and stir, lower the temperature to 25°C, add 22g of succinic acid monoethyl chloride dropwise; after the dropwise ad...

Embodiment 3

[0043] Preparation of red alkali solution: add 50g erythromycin thiocyanate, 140g tetrahydrofuran, and 77g concentration of 20% potassium carbonate solution (w / w) successively in a three-necked flask, heat up to 40°C, and keep warm for 30min; liquid funnel, let stand for stratification, and separate the water layer; transfer the organic layer into a three-necked flask, add 77g of potassium carbonate solution (w / w) with a concentration of 20%, heat up to 40°C, and keep the temperature for 30min; liquid funnel, let stand to separate the layers, separate the water layer, and obtain the red alkali solution, which will be used in the next esterification reaction.

[0044] Preparation of lye: add 3g of sodium bicarbonate and 20g of potassium carbonate to 30ml of water, stir to obtain lye, set aside.

[0045] Add the above lye into the prepared red alkali solution and stir, lower the temperature to 25°C, add 21g of succinic acid monoethyl chloride dropwise, after the addition is comp...

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Abstract

The invention discloses a preparation method of erythromycin ethylsuccinate. The preparation method comprises the following steps of stirring and mixing alkali liquid and berberrubine solution at a proper temperature; then, dripping acyl chloride; performing heat insulation reaction at a proper temperature; performing post treatment; obtaining the erythromycin ethylsuccinate. The preparation method of the erythromycin ethylsuccinate has the advantages that the consumption of esterification reaction acid-binding agents and the alkali liquid is reduced; the production achieves a better environment-friendly effect; the production cost is reduced; the industrial protection is facilitated.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a preparation method of macrolide derivatives, in particular to a preparation method of ethylsuccinate erythromycin. Background technique [0002] Erythromycin Ethylsuccinate is the ethyl succinate of erythromycin, which is widely used clinically in China among many erythromycin derivatives, and is also one of the twenty most commonly used antibacterial drugs in the United States. [0003] The chemical structural formula of erythromycin ethylsuccinate is as follows: [0004] [0005] Xu Qian’s master’s thesis “Research on Production Process Improvement of Erythromycin Ethylsuccinate Based on the Concept of Cost” used potassium carbonate solution with a concentration of 17% as the lye for the esterification reaction. "Research on the Synthesis of Erythromycin Ethylsuccinate" published by Chen Yonghui, "Chemical and Biological Engineering", 2005. NO9; "Research on the Synthetic ...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00
CPCC07H17/08C07H1/00
Inventor 张向阳卢元东汪演华李文辉
Owner HUANGSHI SHIXING PHARMA
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