Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation of good quality benemicin

A rifampicin, high-quality technology, applied in organic chemistry, antibacterial drugs, etc., can solve problems such as high cost and unsatisfactory product quality

Active Publication Date: 2009-07-22
薛荔 +1
View PDF3 Cites 30 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a preparation method of high-quality rifampicin, which solves the problems of unsatisfactory product quality and high cost in traditional preparation methods. Compared with the existing preparation process, it can significantly improve product purity and reduce production costs. It can control the total amount of miscellaneous peaks to less than 1.5%, so that the total consumption of raw materials can be reduced by two-thirds, and the consumption of precious raw material 1-methyl-4-aminopiperazine can be reduced by more than one-half, and the pollution of strong acids and alkalis to the environment can also be eradicated

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0029] The first batch of high-quality rifampicin of the present invention and the operation steps of continuous batch preparation method are as follows:

[0030] Step 1 Salt formation reaction

[0031] In the first batch of production, rifamycin SV was oxidized to generate S, and then extracted with BA to obtain S-BA liquid as the starting material, concentrated to 100,000-140,000 u / ml, from which 50 million units of Add 100-250ml of 6% sodium bicarbonate aqueous solution dropwise to S-BA concentrated feed solution, control 30-50°C for 3-6 hours to generate S sodium salt, cool down to no higher than 10°C to crystallize and filter to obtain the product, and recover the mother liquor To be recycled. It is also possible to directly take the S-BA concentrated feed liquid equivalent to 50 million units of rifamycin S and the recovered mother liquor from the previous batch, repeat the above-mentioned salt-forming reaction, and periodically neutralize the recovered mother liquor wi...

Embodiment 1

[0039] The rifamycin SV is oxidized to generate S, and then extracted with BA to obtain the S-BA feed liquid as the starting material, which is concentrated to 100,000-140,000 u / ml, and the equivalent of 50 million units of S is taken from the concentrated feed liquid Add 150ml of 6% aqueous sodium bicarbonate solution dropwise at 45°C to maintain the reaction for 5 hours. After the reaction is completed, cool down to 10°C for crystallization and suction filtration. The filter cake is washed with pure water and dried, and then dried under reduced pressure at 60°C to obtain S The sodium salt is about 45 grams, and the mother liquor is recovered for recycling. Sodium salt was added to 90ml DMF solution containing 3.8ml acetic acid, stirred at 50°C for 30 minutes to dissociate into S, and then 14.4ml dihydroxy ring was added dropwise to react for 1 hour to obtain oxazine. Recover DMF by molecular distillation, add appropriate amount of ethanol to dissolve it after recovery, and t...

Embodiment 2

[0041] The rifamycin SV is oxidized to generate S, and then extracted with BA to obtain the S-BA feed liquid as the starting material, which is concentrated to 100,000-140,000 u / ml, and the equivalent of 50 million units of S is taken from the concentrated feed liquid Add 150ml of 6% aqueous sodium bicarbonate solution dropwise at 45°C to maintain the reaction for 5 hours. After the reaction is completed, cool down to 10°C for crystallization and suction filtration. The filter cake is washed with pure water and dried, and then dried under reduced pressure at 60°C to obtain S The sodium salt is about 45 grams, and the mother liquor is recovered for recycling. Sodium salt was added to 90ml DMF solution containing 3.8ml acetic acid, stirred at 50°C for 30 minutes to dissociate into S, and then 14.4ml dihydroxy ring was added dropwise to react for 1 hour to obtain oxazine. Recover DMF by molecular distillation, add appropriate amount of ethanol to dissolve it after recovery, and t...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of high-quality rifampicin, solving the problem that the traditional preparation method has the defects such as unfavorable product quality and high cost; the preparation method comprises the operational steps: S-BA liquid is salified by alkalescence sodium bicarbonate during a salification reaction; S is separated out by acetate acid before a cyclization reaction; then, dihydroxy is added for a reaction to obtain oxazine; after the reaction is finished, DMF is recovered by a molecular distillation method and then dissolved by other hydrophilic solvents; oxazine is separated out by an elutriation method; after a hydrolysis reaction and a condensation reaction are finished, an azeotropic distillation method is adopted to recover un-reacted side chains; pH is adjusted and temperature is lowered so that crystals are separated to obtain the crude products of rifampicin; and then the crude products are refined to obtain the high-quality rifampicin. Compared with the existing preparation technique, the preparation method significantly improves the product purity, reduces the production cost, controls the overall quantity of impurities to be lower than 1.5 percent, reduces two thirds of the general consumption of raw materials and more than a half of the usage of 1-methyl-4-aminopyrazine which is a valuable raw material, and eliminates the environmental pollution caused by strong acid and alkali.

Description

technical field [0001] The invention relates to a production process of anti-tuberculosis drugs, in particular to a preparation method for high-quality rifampicin with high quality, low cost and outstanding environmental protection characteristics by using rifamycin SV as a raw material. Background technique [0002] Rifampicin is a semi-synthetic antibiotic of the rifamycin class and is an important anti-tuberculosis drug. According to reports, rifampicin is also a broad-spectrum use of antibiotics, in addition to its high activity against Mycobacterium tuberculosis; Staphylococcus aureus, non-enterococcal streptococcus and Listeria monocytogenes Bacteria, etc. also have high activity; it is also the most effective drug for non-tuberculosis, including tuberculous meningitis. [0003] The preparation method of rifampicin generally adopts the fermentation filtrate of rifamycin SV at home and abroad, and oxidizes it into rifamycin S with a strong oxidant such as ferric chlori...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/08A61P31/06
Inventor 薛守礼薛荔
Owner 薛荔
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com