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

Preparation method of high-purity sulfadoxine

A sulfadoxine, high-purity technology, which is applied in the fields of medicine and chemical industry, can solve the problems of inability to reach, achieve the effect of low cost, small amount of solvent, and outstanding substantive characteristics

Active Publication Date: 2015-04-29
CHONGQING KANGLE PHARMA
View PDF9 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with the advancement of medical science and technology, the daily dose of sulfadoxine is 0.5-1.0 g. According to the regulations on the impurity limit of raw materials in ICH (International Conference on Harmonization of Technical Requirements for Registration of Drugs for Human Use), the maximum daily dose of raw materials is less than 2 g. For pharmaceuticals, the quality control limit for individual impurities is 0.1%. If the products produced by the existing process are tested by high-performance liquid chromatography (HPLC), the single impurity cannot reach ≤0.1%.

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of high-purity sulfadoxine
  • Preparation method of high-purity sulfadoxine
  • Preparation method of high-purity sulfadoxine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1 Sulfadoxine intermediate condensate and finished product HPLC detection method

[0036] Chromatographic conditions:

[0037] Chromatographic column: L11 2.0×10cm, 3μm

[0038] Mobile phase: A: Phosphoric acid aqueous solution (0.1%); B: Acetonitrile (100%) (A:B=83:17)

[0039] Detection wavelength: 230nm

[0040] Flow rate: 0.3ml / min

[0041] Injection volume: 5μl

[0042] Determination method: Take an appropriate amount of this product, accurately weigh 50mg of the sample into a 50ml volumetric flask, first add 5ml of acetonitrile to dissolve, then dilute to the mark with diluent, shake well, and then get it, measure 5μl and inject it into the liquid chromatography, record the chromatogram , calculated according to the peak area normalization method.

Embodiment 2

[0043] The preparation of embodiment 2 sulfadoxine intermediate condensates

[0044]Add 150g of N,N-dimethylformamide into the reaction flask, add 110g of sodium sulfa, and 50g of 4,6-dichloro-5-methoxypyrimidine under stirring, raise the temperature to 88°C-90°C for 3 hours, reduce Pressurize and recover DMF to a temperature of 120°C, add 200g of hot water above 90°C, dissolve completely, adjust the pH to 7.0-8.0 with dilute hydrochloric acid, cool, filter, and use 5% dilute hydrochloric acid to adjust the pH of the filtrate to 3.8-4.1 to precipitate the condensate. Filtration and drying gave 75 g of sulfadoxine intermediate condensate, with a yield of 85.3%. HPLC total impurity: 1.75%, HPLC maximum single impurity: 0.55%. See attached for details figure 1 .

Embodiment 3

[0045] The purification of embodiment 3 sulfadoxine intermediate condensate

[0046] Add 20 g of N,N-dimethylformamide and 20 g of toluene to the reaction flask, add 20 g of the sulfadoxine intermediate condensate (obtained in Example 2) under stirring, heat until dissolved, cool to 0°C to 10°C and keep warm Stir and crystallize for 55-65 minutes, filter and dry to obtain 13.04 g of off-white powder condensate, yield 65.2%, HPLC total impurity: 0.46%, HPLC maximum single impurity: 0.08%. See attached for details figure 2 .

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-purity sulfadoxine, which comprises the following steps: adding a sulfadoxine intermediate condensate crude product into an N,N-dimethylformamide / low-polarity solvent mixed solvent, dissolving by heating, cooling to crystallize to obtain a high-purity sulfadoxine intermediate condensate, carrying out methoxylation reaction to obtain a sulfadoxine crude product, and carrying out conventional acid and alkali refinement on the sulfadoxine crude product to obtain the high-purity sulfadoxine. The method overcomes the defects in the prior art. The method has the following advantages: the HPLC (high performance liquid chromatography) total impurity content of the sulfadoxine is less than 0.4%, and the HPLC maximal single impurity content is less than 0.1%. The whole technique is simple to operate, can obtain the high-quality product, and is suitable for industrialized mass production.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, in particular to a preparation method of high-purity sulfadoxine. Background technique [0002] Sulfadoxine (Sulfadoxine), also known as sulfazone, has a chemical name of 4-(p-aminobenzenesulfonamide)-5,6-dimethoxypyrimidine, and its CAS number is 2447-57-6. Its chemical structure is as follows: [0003] [0004] Sulfadoxine can be used to treat general inflammation clinically, such as upper respiratory tract infection tonsillitis, bacillary dysentery enteritis, skin infection, etc., and can also be compatible with other medicines to treat pulmonary tuberculosis and lymphatic tuberculosis; it also has a certain effect on leprosy (madness). It can also treat malaria, and it can also be used as a preventive medicine for rheumatism. When used for the above purposes, sulfadoxine has the characteristics of long curative effect and low toxicity. After several generations of ...

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): C07D239/69
CPCC07D239/69
Inventor 唐明杨忠鑫黄雪梅秧奇马小平郑雪杨继斌蔡中文
Owner CHONGQING KANGLE PHARMA
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