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Rifamycin S preparing method

A technology of rifamycin and ethanol, which is applied in the direction of organic chemistry, can solve the problems of simple production process, low consumption, and recyclability, and achieve the effects of easy promotion and use, saving production cost and simplifying production process

Inactive Publication Date: 2016-01-13
沈阳抗生素厂
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Adopting isopropanol as solvent in the above method, the addition of isopropanol is 2.15 times of the weight of rifamycin S-Na, compared with the technical scheme disclosed in patent CN102140102A, although this method has reduced raw material consumption to a certain extent, However, it still cannot fully meet the requirements of simple production process, low consumption, recyclability, and less waste.

Method used

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  • Rifamycin S preparing method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation method of this rifamycin S comprises the following steps:

[0025] 1) Using rifamycin S-Na as the starting material, 65vt% ethanol and 95.0~98.0wt% concentrated sulfuric acid as the solvent, under acidic conditions, stir at 40~50°C for 1.5~2h, point the plate during the stirring process, until No rifamycin S-Na spots, the reaction is over;

[0026] Each material mass ratio is rifamycin S-Na: ethanol: purified water: sulfuric acid=100:180:120:8.5;

[0027] 2) Reduce the temperature of the mixture obtained in step 1) to 30°C at a cooling rate of 5°C / h, keep the temperature for 20 minutes, and then drop to room temperature, then lower the temperature to 5°C at a cooling rate of 3°C / h, stop stirring, and let it stand for more than 2 hours , and then centrifuged to obtain a solid mixture and a mother liquor, loosen the crude product of rifamycin S, pickle and wash with water to obtain the crude product of rifamycin S;

[0028] Pickling: Use sulfuric acid to...

Embodiment 2

[0036]In step 1), the mass ratio of each material is rifamycin S-Na:ethanol:purified water:sulfuric acid=100:226:120:9.0, the concentration of ethanol is 70vt%, other steps are the same as in Example 1.

Embodiment 3

[0038] In step 1), the mass ratio of each material is rifamycin S-Na:ethanol:purified water:sulfuric acid=100:145:120:8.0, the concentration of ethanol is 60vt%, and other steps are the same as in Example 1.

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Abstract

A rifamycin S preparing method is characterized by comprising the steps of 1, conducting stirring under the acidic condition for 1.5-2 h with Rifamycin S-Na as the initiator and ethyl alcohol and concentrated sulfuric acid as the solvent, and conducting plate dotting till no Rifamycin S-Na spot exists; 2, cooling the mixture obtained from the step 1 to 5 DEG C, stopping stirring, standing for over 2 h, obtaining a solid mixture and mother liquor through centrifugation, loosening a Rifamycin S crude product, and conducting acid pickling and washing to obtain a Rifamycin S crude product; 3, refining the Rifamycin S crude product obtained from the step 2 to obtain a Rifamycin S refined product; 4, distilling the mother liquor obtained from the step 2 to recover ethyl alcohol to be used in the step 1. The method meets the requirements for simple production process, low consumption, recoverability and low three-waste discharge.

Description

Technical field [0001] The present invention is an organic chemistry field, especially involving a preparation method of a hybrid compound. Specifically, it is a preparation method of Liferrin S. Background technique [0002] Liffunein S, CASNO.13553-79-2, is an important intermediate of synthetic anti-tuberculosis drugs in Lifercin.The main raw materials of spraying ding.Liferrin S is mainly produced with Liferrin S-NA as the starting object. [0003] In the existing technology, the application announcement number CN102140102A has a invention patent application, and the "production method of extracting Liferrin S directly from the fermentation filter fluid from the fermentation filter", including the following steps: ① get from the ilfogencin S.After-washing liquid after washing; ② Tatticate containing olfithromycin S washing into a concentrated tank after washing liquid, controlling the temperature in the concentrated tank does not exceed 50 ° C, decompression concentration, va...

Claims

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Application Information

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IPC IPC(8): C07D498/08
CPCC07D498/08
Inventor 赵德明李治发张岩李卓陈建华张艳影胡亚辉
Owner 沈阳抗生素厂
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