Synthetic technology for ofloxacin

A synthesis process, ofloxacin technology, applied in the field of ofloxacin synthesis process, can solve the problems of reduced yield, long chemical synthesis route, and reduced content of final products, so as to reduce the loss of intermediates and improve the condensation reaction Yield, the effect of reducing the discharge of three wastes

Inactive Publication Date: 2017-09-29
武汉励合生物医药科技有限公司
View PDF5 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Along with the wide use of ofloxacin, its demand grows rapidly, and in the processing route of prior art, because the chemical synthesis route is long, and

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

Example Embodiment

[0019] Example 1

[0020] The present invention provides a synthesis process of ofloxacin, which includes the following steps:

[0021] S1, select (S)-(-)-9,10-difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine[1,2,3-de][1, 4] Phenylazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide as raw materials, and (S)-(-)-9,10-difluoro-2,3-dihydro-3 -Methyl-7oxo-7hydropyridine [1,2,3-de][1,4] phenazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide molar mass The ratio is 1:1:3, and sealed storage;

[0022] S2. Select the reactor as an auxiliary tool, and weigh (S)-(-)-9,10-difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine in proportion to the scale [1 , 2,3-de] [1,4] phenazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide as raw materials, and (S)-(-)-9,10- Difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine[1,2,3-de][1,4]phenazine-6-carboxylic acid, N-methyl Piperazine and dimethyl sulfoxide are sequentially added to the reactor, heated and stirred at 11...

Example Embodiment

[0032] Example 2

[0033] The present invention provides a synthesis process of ofloxacin, which includes the following steps:

[0034] S1, select (S)-(-)-9,10-difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine[1,2,3-de][1, 4] Phenazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide as raw materials, and (S)-(-)-9,10-difluoro-2,3-dihydro-3 -Methyl-7oxo-7hydropyridine [1,2,3-de][1,4] phenazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide molar mass The ratio is 1:1:3, and sealed storage;

[0035] S2. Select the reactor as an auxiliary tool, and weigh (S)-(-)-9,10-difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine in proportion to the scale [1 , 2,3-de] [1,4] phenazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide as raw materials, and (S)-(-)-9,10- Difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine[1,2,3-de][1,4]phenazine-6-carboxylic acid, N-methyl Piperazine and dimethyl sulfoxide are sequentially added to the reactor, heated and stirred for 5 h...

Example Embodiment

[0045] Example 3

[0046] The present invention provides a synthesis process of ofloxacin, which includes the following steps:

[0047] S1, select (S)-(-)-9,10-difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine[1,2,3-de][1, 4] Phenylazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide as raw materials, and (S)-(-)-9,10-difluoro-2,3-dihydro-3 -Methyl-7oxo-7hydropyridine [1,2,3-de][1,4] phenazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide molar mass The ratio is 1:1:3, and sealed storage;

[0048] S2. Select the reactor as an auxiliary tool, and weigh (S)-(-)-9,10-difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine in proportion to the scale [1 , 2,3-de] [1,4] phenazine-6-carboxylic acid, N-methylpiperazine, dimethyl sulfoxide as raw materials, and (S)-(-)-9,10- Difluoro-2,3-dihydro-3-methyl-7oxo-7hydropyridine[1,2,3-de][1,4]phenazine-6-carboxylic acid, N-methyl Piperazine and dimethyl sulfoxide are sequentially added to the reactor, heated and stirred at 13...

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

PropertyMeasurementUnit
Concentrationaaaaaaaaaa
Concentrationaaaaaaaaaa
Concentrationaaaaaaaaaa
Login to view more

Abstract

The invention discloses a synthetic technology for ofloxacin. The synthetic technology comprises the following steps: weighting (S)-(-)-9,10-difluoro-2,3-dihydro-3-methyl-7-oxo-7 hydrogen pyridine (1,2,3-de) (1,4) benzo oxazine-6 carboxylic acid, N-methyl piperazine and dimethyl sulfoxide at a ratio; adding into a reactor in turn; heating, stirring and reacting for 4-8h under the environment at 110-150 DEG C, thereby forming a mixed solution; filtering, adding an alkyl imidazole L-tartrate ionic solution, and heating, stirring and reacting for 30-45min under the environment at 60-80 DEG C; adding an organic solvent, mixing and stirring; reducing pressure and recycling dimethyl sulfoxide and excessive N-methyl piperazine; utilizing 90-95% ethyl alcohol to crystallize the residual solution; and performing hydrolysis reaction, thereby obtaining the ofloxacin. The invention can effectively reduce the happening of side reaction and can increase the yield of condensation reaction.

Description

technical field [0001] The invention relates to the technical field of compound synthesis, in particular to a synthesis process of ofloxacin. Background technique [0002] Ofloxacin, yellowish crystalline powder; odorless, bitter taste; gradually changing color when exposed to light. This product is slightly soluble in chloroform, slightly soluble in methanol, easily soluble in glacial acetic acid, slightly soluble in dilute acid and 0.1mol / L sodium hydroxide solution. The main component of ofloxacin hydrochloride is ofloxacin. Its chemical name is: (S)-(-)-9-fluoro-2,3-dihydro-3-methyl-10-(4-methyl-1-piperazinyl)-7-oxo-7H - Pyrido[1,2,3-de]-[1,4]benzoxazine-6-carboxylic acid hemihydrate. Molecular formula: C18H20FN3O4·1 / 2H2O, molecular weight: 370.38. [0003] Along with the wide use of ofloxacin, its demand grows rapidly, and in the processing route of prior art, because the chemical synthesis route is long, and the unreacted intermediate is easy to react with aminopro...

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
IPC IPC(8): C07D498/06
CPCC07D498/06
Inventor 彭凡李娜田军叶杨欢叶志伟
Owner 武汉励合生物医药科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap