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

Novel method for refining aripiprazole

A technology of aripiprazole and aripiprazole salt, applied in the direction of organic chemistry and the like, can solve the problems of low refining yield, difficult post-processing, low solubility, etc., and achieve the effect of high yield and purity

Inactive Publication Date: 2012-08-01
北京德众万全医药科技有限公司
View PDF6 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, the disadvantage of this route is that there are more reactive sites, and it is easy to produce more by-products, such as:
If refining is carried out in the first step, the patent US20100130744 provides a refining method using a toluene-silica gel system for refining. Our verification shows that this method can effectively reduce the content of impurity ⅡA, but the refining yield is low, greatly Reduced effective utilization of the product
At the same time, due to the low solubility of intermediate II in toluene, the liquid-solid ratio of the solvent used in the purification exceeds 40:1, the amount of solvent used is large, and the post-treatment is difficult, which is not suitable for industrial operation.

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
  • Novel method for refining aripiprazole
  • Novel method for refining aripiprazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 20 g of crude aripiprazole and 120 mL of acetone into a 250 mL three-necked flask, stir, and heat to reflux. Add 20 mL of concentrated hydrochloric acid, stir for half an hour, and filter with suction. Dissolve the filter cake in 300 mL N,N-dimethylformamide, stir under temperature control, and gradually add 5% NaOH aqueous solution dropwise to control the pH=8.5~9, filter with suction, wash the filter cake with distilled water until neutral , and dried at 40 ℃ to obtain 16 g of white aripiprazole crystals with a yield of 80%.

Embodiment 2

[0021] Add 20 g of crude aripiprazole and 120 mL of tetrahydrofuran into a 250 mL three-necked flask, stir, and heat to reflux. Add 20 mL of concentrated hydrochloric acid, stir for half an hour, and filter with suction. Dissolve the filter cake in 300 mL N,N-dimethylformamide, stir at constant temperature, and gradually add 1% KOH aqueous solution dropwise to control the pH=8.5-9, filter with suction, wash the filter cake with distilled water until neutral, After drying at 40 °C, 17.5 g of white aripiprazole crystals were obtained, with a yield of 87.5%.

Embodiment 3

[0023] Add 40.0 g of crude aripiprazole and 350 mL of ethanol into a 500 mL three-necked flask, stir, and heat to reflux. Slowly add 16.0 g oxalic acid, stir for half an hour, cool, and filter with suction. Dissolve the filter cake in 500 mL N,N-dimethylformamide, stir at constant temperature, and gradually add 5% NaOH aqueous solution dropwise to pH=8.5~9, filter with suction, wash the filter cake with distilled water until neutral , and dried at 40 ℃ to obtain 32.8 g of white aripiprazole crystals with a yield of 82%.

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 provides a method for refining aripiprazole. By using the salifying and recrystallization combined technique, the method can be used for preparing the high-purity aripiprazole product in a simple and efficient way.

Description

technical field [0001] The invention provides a method for refining aripiprazole. The method can obtain the aripiprazole product with high purity more concisely and efficiently by using the combination technology of salt formation, desalination and recrystallization. Background technique [0002] Aripiprazole, the chemical name is 7-[4-[4-(2,3-dichlorophenyl)-1-piperazinyl]butoxy]-3,4-dihydroquinolinone, and its chemical The structural formula is: [0003] [0004] Aripiprazole belongs to quinolone derivatives, and it is a psychoneuropharmaceutical used for the treatment of schizophrenia such as panic, obsessive-compulsive disorder, sleep disorder, sexual dysfunction, depression, anxiety or mania (US5006528, US4734416). Approved for listing in several countries. [0005] Regarding the synthesis of aripiprazole, several patents (EP367141, US5006528, CN1028104C, CN1042537A) describe the following synthesis methods. [0006] The reaction route is short, the source of r...

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): C07D215/227
Inventor 王晓璐宋雪梅郭夏
Owner 北京德众万全医药科技有限公司
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