Method for preparing erythromycin thiocyanate

A technology of erythromycin thiocyanate and erythromycin, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve problems such as affecting product quality stability and product quality fluctuations.

Active Publication Date: 2012-10-17
TOPFOND PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing technology all adopts the method of primary crystallization when forming salt crystallization.
In the actual operation process, due to the cha...

Method used

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  • Method for preparing erythromycin thiocyanate
  • Method for preparing erythromycin thiocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 100350530 batches of erythromycin extract 2T after washing (potency 35862u / ml, components A96.3%, B2.5%, C1.2%), and heat to 38°C. According to the calculation of 1.5L / billion, 107.6L of 15% sodium thiocyanate solution should be added. The first salt crystallization: first add 36L of 15% sodium thiocyanate solution, start stirring, slowly add 15% acetic acid solution, adjust the pH to 8.0 to form salt crystallization. After 20 minutes, the crystallization solution was separated by vacuum filtration. After being drained, rinse with a small amount of new ethyl acetate and drain. Then soak and wash with purified water at 55°C, then drain and vacuum dry to obtain 20.10Kg of finished product, with a billion yield of 27.3%, components A80.2%, B2.5%, and C1.4%; the second time Salt formation and crystallization: maintain the separated crystallization mother liquor at 38°C, add 71.6L of 15% sodium thiocyanate solution, start stirring, slowly add 15% acetic acid solution,...

Embodiment 2

[0029] Take 100350560 batches of erythromycin extract 2T after washing (potency 36570u / ml, components A94.2%, B3.6%, C2.2%), and heat to 35°C. According to the calculation of 1.2L / billion, 87.76L of 20% sodium thiocyanate solution should be added. The first salt crystallization: first add 21.9L of 15% sodium thiocyanate solution, start stirring, slowly add 15% acetic acid solution, and adjust the pH to 8.2 to form salt crystallization. After 20 minutes, the crystallization solution was separated by vacuum filtration. After being drained, rinse with a small amount of new butyl acetate and drain. Then soak and wash with purified water at 55°C, then drain and vacuum-dry to obtain 19.82Kg of finished product, with a yield of 25.7% per billion, and components A78.1%, B2.7%, and C1.8%; the second time Salt formation and crystallization: maintain the separated crystallization mother liquor at 36°C, add 65.86L of 20% sodium thiocyanate solution, start stirring, slowly add 15% acetic...

Embodiment 3

[0031] Take 100350580 batches of erythromycin extract 2T after washing (potency 37605u / ml, components A97.1%, B1.9%, C1.0%), and heat to 40°C. According to the calculation of 1.3L / billion, 97.8L of 18% sodium thiocyanate solution should be added. The first salt crystallization: first add 31.2L of 15% sodium thiocyanate solution, start stirring, slowly add 15% acetic acid solution, and adjust the pH to 8.0 to form salt crystallization. After 20 minutes, the crystallization solution was separated by vacuum filtration. After being drained, rinse with a small amount of new butyl acetate and drain. Then soak and wash with purified water at 55°C, then drain and vacuum-dry to obtain 26.33Kg of finished product, the yield per billion is 28.5%, and components A80.4%, B2.1%, and C1.2%; the second time Salt formation and crystallization: maintain the separated crystallization mother liquor at 40°C, add 66.6L of 18% sodium thiocyanate solution, start stirring, slowly add 15% acetic acid...

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Abstract

The invention provides a method for preparing erythromycin thiocyanate, which uses a secondary crystallization method, the process is simple, no device is required, the quality of the erythromycin thiocyanate products can be partially increased, and the product quality fluctuation caused by change of quality of fermentation liquid can be overcome.

Description

technical field [0001] The invention relates to a preparation method of macrolide antibiotics, in particular to a preparation method of erythromycin thiocyanate. Background technique [0002] Erythromycin Thiocyanate, a macrolide antibiotic, is the thiocyanate of erythromycin, a white or off-white crystalline powder or loose block. This product is used for the infection of Gram-positive bacteria and mycoplasma; it is more used for the synthesis of macrolide antibiotics such as erythromycin ethylsuccinate, roxithromycin, azithromycin, odorless erythromycin, and clarithromycin. In recent years, the export of erythromycin thiocyanate has shown a continuous upward trend, especially in 2008 and 2009, the export increased by 18% and 25% respectively year-on-year, becoming a variety with a relatively high increase in the intermediates of similar antibiotics. At the same time, its price is also on the rise, but the market is still in short supply. However, due to technical reasons...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/00
Inventor 李武德刘守强张宏周毛全贵宋喜芳陈忠刚杨琳琳董易凡李磊林恒标巩新玉李翠平
Owner TOPFOND PHARMA CO LTD
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