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A kind of hydrolysis method of pleuromutilin

A technology for pleuromutilin and hydrolyzate, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve problems such as large environmental pollution and complicated product processing, and achieve high product yield and production efficiency. The effect of short cycle and reduced usage

Active Publication Date: 2015-11-18
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a variety of organic solvents, the product treatment is relatively complicated, and the environmental pollution is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Slowly add 2 times the volume of sulfuric acid aqueous solution with a concentration of 1mol / L to the pleuromutilin butyl acetate extract with a mass volume concentration of 10%, and raise the temperature to 80°C for 6 hours under stirring; after the reaction is completed, let it stand Separate the layers, discard the water phase, concentrate the upper butyl acetate phase in vacuum at 65°C, add hot water 0.5 times the volume of the concentrated solution, and wash twice. After washing, add anhydrous sodium sulfate to dehydrate, and filter; The temperature of the solution was slowly lowered to 0°C, the product was precipitated, filtered and dried to obtain the hydrolyzed product of pleuromutilin. Yield 94%, purity 92.4%.

Embodiment 2

[0022] Slowly add 2 times its volume, 1.5 mol / L sulfuric acid aqueous solution to the 12% pleuromutilin butyl acetate extract, stir and raise the temperature to 90°C for 6 hours; layer, discard the water phase, concentrate the upper butyl acetate phase in vacuum at 70°C, add hot water 1 times the volume of the concentrated solution to wash 3 times, add anhydrous sodium sulfate to dehydrate, and filter; the filtrate Slowly lower the temperature to 0°C, the product precipitates, and is filtered and dried to obtain pleuromutilin hydrolyzate. Yield 90%, purity 93.7%.

Embodiment 3

[0024] Slowly add 3 times its volume, 2mol / L sulfuric acid aqueous solution to the pleuromutilin butyl acetate extract with a mass volume concentration of 15%, and heat up to 80°C for 5 hours under stirring; after the reaction is completed, let stand and separate , discard the water phase, vacuum concentrate the upper butyl acetate phase at 70°C, add hot water 1 times the volume of the concentrated solution to wash 3 times, add anhydrous calcium chloride for dehydration after washing, and filter; the filtrate Slowly lower the temperature to 5°C, the product precipitates, and is filtered and dried to obtain the pleuromutilin hydrolyzate. Yield 89%, purity 95.6%.

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Abstract

A hydrolysis method for pleuromutilin comprises: adding a sulfuric acid aqueous solution into an butyl acetate extracting solution of pleuromutilin, heating to 80-90 DEG C with stirring, reacting for 5-6 h; after the reaction is finished, standing for layering, performing vacuum concentration at 65 DEG C-70 DEG C on the supernatant butyl acetate phase; washing the concentrated solution with hot water for 2-3 times, then adding a drying agent for dehydration, and filtering; and slowly cooling the filtrate to 0-5 DEG C, precipitating the product, and filtering and drying to obtain the pleuromutilin hydrolysis product. The low-concentration sulfuric acid aqueous solution is employed for hydrolysis of pleuromutilin, strong alkalis are avoided, the operation risk is reduced; the method employs direct concentrating crystallization and does not introduce a second solvent, so that the organic solvent is reduced for usage; and the production period is relatively short, the operation is simple, the product yield is relatively high, pollution is relatively less, and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to the technical field of biological fermentation, in particular to a method for hydrolyzing pleuromutilin. Background technique [0002] Pleuromutilin is a diterpenoid veterinary antibiotic produced by higher fungi, which has strong antibacterial activity against Gram-positive bacteria and mycoplasma. The structure-activity relationship study of pleuromutilin shows that its C-14 side chain has good biological activity, and modification of the C-14 side chain can change its activity. At present, derivatives of pleuromutilin have been successfully developed at home and abroad, such as tiamulin, valnemulin, retapamulin and azamulin. Through chemical modification, the antibacterial activity of this type of antibiotics is obviously improved, and has a good application prospect. [0003] At present, the domestic production of pleuromutilin derivatives all adopts high-yield pleuromutilin fungus fermentation to prepare pleuromutilin fe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/743C07C45/64C07C59/06C07C51/09
CPCC07C45/65C07C51/09C07C2603/82C07C49/743C07C59/06
Inventor 王义周丽娜
Owner 宁夏泰瑞制药股份有限公司
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