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Organic solvent and extraction method for extracting crude product of pleuromutilin

A technology of pleuromutilin and organic solvents, which is applied in the fields of organic chemistry, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of many times of extraction, long production cycle, and high market price, so as to shorten the production cycle, The effect of improving production efficiency and strengthening market competitiveness

Pending Publication Date: 2017-05-10
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1 The extraction times are many, generally 2-3 times, resulting in a long production cycle, more than 10 hours, and low production efficiency
[0005] 2 The flash drying process is used in the extraction process, which consumes a lot of energy
[0006] 3 The pleuromutilin residue is prone to odor during the flash drying process, which brings pressure on the environmental protection of enterprises
[0007] 4. The organic solvent MIBK or acetone is used in the extraction process of pleuromutilin fungus residue. Due to its high market price, the extraction cost is high
[0008] 5 Domestic related literatures reported that a single organic solvent was used to extract pleuromutilin residues, and the extraction yield was relatively high. However, it was verified by experiments that the total yield was generally 90-95%, and some pleuromutilins were not completely Extracted and applied to large-scale industrial production, the amount of organic solvent used is large, which has a certain impact on environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Pleuromutilin Fermentation Broth 10m 3 , the potency is 20473u / ml, 2.7 tons of pleuromutilin wet slag obtained by plate and frame filtration, adding 0.54 tons of drinking water for washing, and filtering to obtain 2.6 tons of pleuromutilin wet slag after washing.

[0033] Add organic solvent, N,N-dimethylformamide 2.6m to the wet pleuromutilin residue 3 , the temperature was raised to 30°C, the leaching time was 100min, and the stirring speed was controlled at 90r / min. After the leaching is finished, filter to obtain pleuromutilin solution 3.1m 3 .

[0034] Add 0.52 tons of montmorillonite to the pleuromutilin solution, and then filter to obtain pleuromutilin organic solution 2.5m 3 .

[0035] The pressure was controlled at -0.05 MPa, the temperature of the pleuromutilin solution was raised to 145°C, and N,N-dimethylformamide was collected; after the concentration under reduced pressure, 201 kg of solid pleuromutilin was obtained with a yield of 99.1%.

Embodiment 2

[0037] Pleuromutilin Fermentation Broth 10m 3 , the potency is 20186u / ml, 2.5 tons of pleuromutilin wet slag obtained by plate and frame filtration, 0.75 tons of drinking water is added, and 2.6 tons of pleuromutilin wet slag are obtained by filtration after washing.

[0038] Add organic solvent, N,N-dimethylformamide 5.2m to the wet pleuromutilin residue 3 , the temperature was raised to 32°C, the leaching time was 120min, and the stirring speed was controlled at 95r / min. After the leaching is finished, filter to obtain pleuromutilin solution 5.1m 3 .

[0039] Add 0.572 tons of cellulose to the pleuromutilin solution, then filter to obtain pleuromutilin organic solution 5.1m 3 .

[0040] The pressure was controlled at -0.07MPa, and the temperature of the pleuromutilin solution was raised to 148°C, and N,N-dimethylformamide was collected; after concentrating under reduced pressure, 198.8kg of solid pleuromutilin was obtained with a yield of 99.5%.

Embodiment 3

[0042] Pleuromutilin Fermentation Broth 10m 3 , the potency is 20247u / ml, 2.8 tons of pleuromutilin wet slag obtained by plate and frame filtration, 1.12 tons of drinking water are added, and 2.5 tons of pleuromutilin wet slag are obtained by filtration after washing.

[0043] Add organic solvent, N,N-dimethylformamide 7.5m to the wet pleuromutilin residue 3 , the temperature was raised to 35°C, the leaching time was 150min, and the stirring speed was controlled at 100r / min. After the leaching is finished, filter to obtain pleuromutilin solution 7.6m 3 .

[0044] Add 0.6 tons of montmorillonite to the pleuromutilin solution, and then filter to obtain pleuromutilin organic solution 7.5m 3 .

[0045] The pressure was controlled at -0.1MPa, the temperature of the pleuromutilin solution was raised to 150°C, and N,N-dimethylformamide was collected; after the concentration under reduced pressure, 199.2kg of solid pleuromutilin was obtained with a yield of 99.4%.

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PUM

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Abstract

The invention relates to an organic solvent and an extraction method for extracting a crude product of pleuromutilin. The organic solvent is the mixture of N,N-dimethyl formamide or / and butyl ether, ethanol and butanol. The method comprises the following steps of first water-scrubbing the wet fungus residue, which is obtained through being filtered through a plate frame, of the pleuromutilin, adding the wet fungus residue of the pleuromutilin into the organic solvent for lixiviating, and filtering an obtained mixture, so as to obtain the crude product of the pleuromutilin through drying and vacuum concentration. By using the organic solvent and the extraction method, the lixiviation yield of the pleuromutilin is obviously improved; the extraction period is shortened; the energy consumption and the cost are decreased; the environmental-protection pressure is eased; the organic solvent and the extraction method are applicable to industrialized production.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction, and in particular relates to an organic solvent and an extraction method for extracting crude pleuromutilin. Background technique [0002] Pleuromutilin is a kind of broad-spectrum diterpene antibiotic produced by the fermentation of Pleuromutilus. It was first isolated and reported its activity in 1951. At present, the pleuromutilin antibiotics developed and marketed in the international market are all pleuromutilin derivatives, among which tiamulin and warnimulin have been listed as veterinary drugs, and the pleuromutilin developed and produced by GlaxoSmithKline in 2007 Retapamulin is the first pleuromutilin antibiotic approved by the FDA for human use. So far, scholars at home and abroad have focused on the synthesis of new derivatives, with the goal of developing new human antibiotics with better water solubility and better pharmacokinetic properties and low drug resistance. ...

Claims

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Application Information

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IPC IPC(8): C07C67/48C07C67/56C07C67/58C07C69/675
CPCC07C67/48C07C67/56C07C67/58C07C69/675
Inventor 任勇
Owner 宁夏泰瑞制药股份有限公司
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