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

Purification method of sertaconazole nitrate

A kind of technology of sertaconazole nitrate and purification method, applied in the field of purification of sertaconazole nitrate, can solve problems such as different melting points

Pending Publication Date: 2021-10-15
HAINAN HAISHEN TONGZHOU PHARM CO LTD
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the melting point of sertaconazole nitrate recorded in the European Pharmacopoeia or the British Pharmacopoeia is 156-161°C, which is obviously different from the melting point recorded in the Chinese drug standards

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
  • Purification method of sertaconazole nitrate
  • Purification method of sertaconazole nitrate

Examples

Experimental program
Comparison scheme
Effect test

preparation example

[0034] (1) 80kg purified water is added in the reaction kettle, open and stir, add 2.92kg sodium hydroxide while stirring, make it dissolve completely, obtain 3.6wt% sodium hydroxide solution, then add 10.4kg o-chlorothiophenol, stir at room temperature 30min; add 6.66kg of chloroacetone under stirring, and then stir for another 60min to react. Then add 21.36kg ether to extract the aqueous layer, and wash with water 3 times. The ether layer was collected in separate layers, combined with the oil layer and then distilled under reduced pressure to recover the ether to obtain 12.14 kg of o-chlorophenylthioacetone.

[0035] (2) Add 121.4kg of polyphosphoric acid in reactor A, stir, then add 12.14kg of o-chlorophenylthioacetone, heat up to 120°C and start to keep warm for 5 hours, and control the temperature at 120-140°C. Add water in another reaction kettle B, and cool down for later use. Release the reaction liquid in the reactor A, and slowly add it to another reactor B for di...

Embodiment 1

[0040] Add 60.63 g of 95% ethanol into the reaction flask, stir, heat, and raise the temperature to 60° C., add 23.04 g of crude sertaconazole nitrate while stirring, and heat up to reflux for 1 hour. Add activated carbon, reflux for 15 minutes, and filter the activated carbon while it is hot. The filtrate was added dropwise with 60.63 g of purified water under stirring, and crystals were precipitated. After the dropwise addition was completed, the mixture was stirred for another 30 minutes and filtered to obtain crystals. Dry in a vacuum oven to obtain 19.06 g of sertaconazole nitrate finished product.

Embodiment 2

[0042] The difference between embodiment 2 and embodiment 1 is that the consumption of 95% ethanol is 100g.

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 purification method of sertaconazole nitrate, which is characterized by being used for preparing a sertaconazole nitrate crystal form with a melting point of 156-161 DEG C. The purification method comprises the following steps: (1) mixing a sertaconazole nitrate crude product with 95% ethanol, heating and refluxing; (2) adding activated carbon, and then continuously refluxing; (3) after the reflux is finished, filtering to remove the activated carbon to obtain filtrate; (4) dropwise adding water into the obtained filtrate while stirring, and separating out crystals; and (5) after dropwise adding, filtering and drying the crystal. According to the purification method of sertaconazole nitrate provided by the invention, after the crude product of sertaconazole nitrate is heated and dissolved by using 95% ethanol, water is dropwise added for solventing-out crystallization, and it is accidentally found that a sertaconazole nitrate crystal form with the melting point of 156-161 DEG C can be obtained. The melting point of the crystal form meets the requirements of European Union Pharmacopoeia or British Pharmacopoeia, and technical support is provided for exporting drugs to the countries and regions.

Description

technical field [0001] The invention relates to the technical field of preparation of raw materials, in particular to a purification method of sertaconazole nitrate. Background technique [0002] Sertaconazole nitrate is a synthetic imidazole broad-spectrum antifungal drug, which can inhibit and kill dermatophytes, yeasts, candida, and aspergillus, and has strong antibacterial effects on Gram-positive bacteria. [0003] For the purification of sertaconazole nitrate crude drug, the prior art generally adopts 95% ethanol to heat and dissolve the crude sertaconazole nitrate, then cool down and stand for crystallization to recrystallize it. The inventors found that by adopting this recrystallization method, the melting point of the obtained sertaconazole nitrate is 163-167° C., which meets the requirements of the National Drug Standards of the State Food and Drug Administration of China. [0004] However, the melting point of sertaconazole nitrate recorded in the European Pharm...

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): C07D409/12
CPCC07D409/12C07B2200/13
Inventor 刘玉韦家华李博福
Owner HAINAN HAISHEN TONGZHOU PHARM CO LTD
Features
  • Generate Ideas
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com