Azithromycin amine crystallization method

A technology of azithromycin amine and crystallization, applied in the field of crystallization of azithromycin amine, can solve the problems of difficult preservation, dangerous production process, fast degradation speed of azithromycin amine, etc., achieves simple operation and process control, reduces the influence of product quality, and reduces solvent The effect of the recycling process

Pending Publication Date: 2022-05-20
SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD
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Problems solved by technology

The whole operation process is cumbersome, the process takes a long time, and the stability of the final azithromycin amine is poor, and the degradation speed of azithromycin amine is fast; the acetone used in the process is a flammable and explosive control reagent, which causes danger in the production process and difficulty in storage. And because of the volatile characteristics of acetone, the recovery rate is low, which increases the preparation cost

Method used

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  • Azithromycin amine crystallization method

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Embodiment Construction

[0022] The following technical solution is described in detail in conjunction with an embodiment of the present invention, the present invention discloses a crystallization method of azithromycin. The preparation of azithromycin acid aqueous phase is carried out first, and then the aqueous phase of azithromycin is reacted with azithromycin, and the solid-liquid separation is carried out by taking advantage of the water-insoluble nature of the generated azithromycin. Its reaction formula is as follows:

[0023]

[0024] The crystallization steps are described below:

[0025]Add 2300L of drinking water to the chloroform phase of azithromycin, cool down to 0~ 10 °C; add 32% hydrochloric acid dropwise to adjust the pH of 4.5 to 5, stir for 10 to 20 min and then stand for 20 to 30 min, split into phases, separate out of the aqueous phase of azithromycin acid; add 3000L of water to the crystallization tank, heat up to 55 °C. Since azithromycin is unstable in acidic or alkaline cases, ...

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Abstract

The invention provides a crystallization method of azithromycin amine. The method comprises the following steps: preparing an azithromycin amine water phase, reacting ammonia water with the azithromycin amine water phase, and carrying out solid-liquid separation by utilizing the characteristic that generated azithromycin amine is insoluble in water to obtain final azithromycin amine. No solvent is used in the crystallization process, the solvent consumption is reduced, meanwhile, the safety coefficient in the generation process is improved, the concept of green chemical development is better met, and the solvent recovery procedure can be reduced; the production cost is saved, the equipment utilization rate is improved, the operation and process control are simpler and more convenient, and the influence of process operation problems on the product quality is reduced.

Description

Technical field [0001] The present invention relates to the field of organic chemistry techniques, specifically to a crystallization method of azithromycin. Background [0002] Azithromycin, chemical name 9-deoxy-9a-aza-9a-erythromycin A, its structural formula is as follows, is an intermediate of azithromycin, the prior art in the preparation of azithromycin is mainly by azithromycin chloroform phase, first by acid extraction to the aqueous phase, partially added to the bottom liquid of acetone and ammonia, and then add ammonia, and finally add the remaining azithromycin aqueous phase, until the drip is added, cooling crystallization, flinging, to obtain azithromycin. The whole operation process is cumbersome, the process takes a long time, and the stability of the final preparation of azithromycin is poor, and the degradation rate of azithromycin is fast; the acetone used in the process belongs to the flammable and explosive regulatory reagents, resulting in the production proc...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07H17/08C07H1/06
Inventor 昝日虎白晶王启斌卢方洲
Owner SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD
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