Refining method for propofol injection

A dipropofol and rectification technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of high temperature, harsh conditions, high production equipment requirements, etc., to avoid damage and mild production conditions , The effect of simple production and operation

Active Publication Date: 2007-12-05
XIAN LIBANG PHARMA
View PDF0 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high requirements on production equipment, harsh conditions and high temperature

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
  • Refining method for propofol injection
  • Refining method for propofol injection
  • Refining method for propofol injection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Description of refining process

[0027] Referring to Figure 1, put 5g~8g of 200-300 mesh silica gel into a Φ18mm×200mm chromatography column, put a little clean sand on the upper layer of silica gel, and install it.

[0028] Draw 1.0 g of crude dipropofol with a purity of 98.33% with a straw, and slowly flow the sample down along the inner wall of the chromatographic column near the sand layer in a circle. Slowly add the eluent petroleum ether (or n-hexane) along the inner wall of the column, open the cock of the chromatography column, start elution and add eluent successively (pressurization can be used to speed up the elution speed). The elution process was monitored by thin-layer chromatography, the main fraction (about 1.0-1.5 L) was collected, concentrated with a rotary thin film evaporator, and the solvent was evaporated to dryness to obtain 0.9 g of the product, with a yield of 91.5%. Testing (including bacterial testing and product quality analysis) fully m...

Embodiment 2

[0059] Put 500g~800g, 200mesh~300mesh silica gel into a Φ65mm×800mm chromatography column, put a little clean sand on the upper layer of silica gel, and install it. Slowly and evenly add 100.0 g of crude dipropofol with a purity of 91.7% along the inner wall of the chromatography column. Slowly add the eluent petroleum ether along the inner wall of the column, open the cock of the chromatography column, start elution and add eluent successively (pressurization can be used to speed up the elution speed). Use TLC to monitor the elution process, collect the main fraction (about 8-15 L), concentrate with a rotary thin film evaporator, evaporate the solvent to dryness, and obtain 82.6 g of the finished product, with a yield of 90.0%. Testing (including bacterial testing and product quality analysis) fully meets the requirements of the USP28 standard, and the purity is 99.93%. Then packed with nitrogen and stored at low temperature. The purity analysis method and structure determi...

Embodiment 3

[0061] Put 5kg~8kg, 200mesh~300mesh silica gel into a Φ160mm×1600mm chromatography column, and install it. Slowly and evenly add 1.0 kg of crude dipropofol with a purity of 83.4% along the inner wall of the chromatography column. Slowly add the eluent n-hexane along the inner wall of the column, open the cock of the chromatography column, start elution and add eluent successively (pressurization can be used to speed up the elution speed). The elution process was monitored by TLC, the main fraction (about 60-100 kg) was collected, concentrated by a rotary thin film evaporator, and the solvent was evaporated to dryness to obtain 743 g of the finished product with a yield of 89.1%. Testing (including bacterial testing and quality analysis of finished products) fully meets the requirements of the USP28 standard, and the purity is 99.94%. The purity analysis method and structure determination are the same as in Example 1.

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 present invention discloses bipropofol refining process, which includes chromatographic column separation to eliminate impurities with similar chemical structures, and rectification in a rotary film evaporator with shortened detention period of the material in the heating evaporation region and reduced thermal decomposition of bipropofol. The process of the present invention is superior to available refining processes, and has short refining period, less degradation of bipropofol and high product quality controllability.

Description

technical field [0001] The invention relates to a method for refining the compound propofol, in particular to a method for refining dipropofol. Background technique [0002] Dipropofol is currently the most ideal and excellent anesthetic drug for clinical application, and its chemical structural formula is: [0003] [0004] However, the synthesis of dipropofol will produce many other compounds with very similar structures. In addition, dipropofol is very easily oxidized, which makes the separation and purification of dipropofol difficult. [0005] At present, the more effective separation methods are low temperature recrystallization and double-step rectification. Low-temperature recrystallization utilizes the difference in solubility of dipropofol and other impurities in non-polar solutions at low temperature to selectively crystallize dipropofol at low temperature. Because the operating conditions of dipropofol low-temperature crystallization ...

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): C07C39/06C07C37/70
Inventor 陈涛王进关京钢
Owner XIAN LIBANG PHARMA
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