Sevoflurane synthesizing method

A sevoflurane, a new synthesis technology, applied in ether preparation, organic chemistry and other directions, can solve the problems of decreased yield and purity, unsuitable for industrial production, raw materials need to be recovered, etc., and achieves easy operation, easy control of reaction conditions, and three wastes discharge. less effect

Active Publication Date: 2009-03-11
福安药业集团重庆博圣制药有限公司 +1
View PDF15 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it is disclosed in these two patent international applications that concentrated sulfuric acid, hexafluoroisopropanol, formaldehyde equivalents, and chlorinating reagents are reacted together to obtain chloromethyl ether, but Ogari Pacheco limits the chlorinating reagents to oxalyl chloride, tris Phosphorus chloride, phosphorus pentachloride, phosphorus oxychloride, and thionyl chloride; in addition, Ogari Pacheco et al. believe that the reaction is carried out under atmospheric humidity conditions, and aluminum trichloride is a very hygroscopic solid. Lower the yield an...

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
  • Sevoflurane synthesizing method
  • Sevoflurane synthesizing method
  • Sevoflurane synthesizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Add 400 g of hexafluoroisopropanol, 84 g of paraformaldehyde and 30 ml of concentrated sulfuric acid into a 500 ml flask, stir and heat to 45-50° C., react for 2 hours, stop stirring, cool down to room temperature, and set aside for later use.

[0066] 300.0 g of sevoflurane crude product and 340 g of anhydrous aluminum trichloride were added to a 3000ml three-necked flask, cooled to 0 °C, and the reaction solution for use in Example 1 was added dropwise with stirring, and the temperature of the reaction solution was controlled not to exceed 10 °C. After completion of the reaction at 0 °C for 0.5 hours, heating to 25-30 °C, after 10 hours of reaction, 1000 ml of polyethylene glycol was added, 232 g of anhydrous potassium fluoride was added with stirring, and the reaction was heated and refluxed under normal pressure for 4 hours; All fractions were collected to obtain 661.5 g of crude sevoflurane (GC 97.36%, yield 70.1%). The crude product was rectified to obtain 584.7 g...

Embodiment 2

[0068] Add 400 g of hexafluoroisopropanol, 84 g of paraformaldehyde, and 40 ml of concentrated sulfuric acid into a 500 ml flask, stir and heat to 45-50 ° C, react for 2 hours, stop stirring, cool down to room temperature, and separate the lower layer of concentrated sulfuric acid for later use.

[0069] 300.0 g of sevoflurane crude product and 340 g of anhydrous aluminum trichloride were added to a 3000ml three-necked flask, cooled to 0 °C, and the reaction solution for use in Example 1 was added dropwise with stirring, and the temperature of the reaction solution was controlled not to exceed 10 °C. After completion of the reaction at 0 °C for 0.5 hours, heating to 25-30 °C, after 10 hours of reaction, 1000 ml of polyethylene glycol was added, 232 g of anhydrous potassium fluoride was added with stirring, and the reaction was heated and refluxed under normal pressure for 4 hours; All fractions were collected to obtain 676.5 g of crude sevoflurane (GC 97.36%, yield 73.2%). The...

Embodiment 3

[0072] Add 300.0 g of sevoflurane crude product, 340 g of anhydrous aluminum trichloride, 400 g of hexafluoroisopropanol, and 84 g of paraformaldehyde into a 3000-ml three-necked flask, cool down to 0 °C, and add 40 ml of concentrated sulfuric acid dropwise with stirring to control the reaction solution. The temperature does not exceed 10 °C, after the addition is completed, the reaction is carried out at 0 °C for 0.5 hours, and the temperature is heated to 25-30 °C. After 10 hours of reaction, 1000 ml of polyethylene glycol is added, and 232 g of anhydrous potassium fluoride is added with stirring, and the reaction is heated and refluxed under normal pressure. 4 hours; atmospheric distillation, collecting all fractions to obtain a total of 636.5 g of crude sevoflurane (GC 97.36%, yield 65.3%). The crude product was rectified to obtain 542.3 g of sevoflurane (GC 99.998%, yield 85.2%).

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 method for applying methylating halogen, which is a new method to use hexafluoro isopropanol, formaldehyde equivalent, strong acid, alchlor and metal fluoride as raw materials to react so as to synthesize high-purity and high-yield sevoflurane. The method is characterized in that the reaction condition is easy to control without unnecessary intermediate processes of separation and purification, the post-treatment is simple, mostly raw materials and auxiliary materials can be recovered and used repeatedly so that the yield of the 'three wastes' is quite little, the product yield is high, the production time of single batch is shortened greatly, and the production efficiency is improved, thus the method is applicable to large-scale industrial production.

Description

technical field [0001] The present invention relates to a synthetic method of inhalable anesthetics, more particularly, to a new synthetic method of sevoflurane. Background technique [0002] Sevoflurane, chemical name: fluoromethyl 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether, was first approved in the United States in 1995 for inhalation anesthesia for induction and maintenance of general anesthesia medicine. [0003] Since sevoflurane is an α-fluoroalkyl ether, there are many difficulties in its chemical synthesis, among which different synthesis techniques often lead to low yields, different by-products, and harsh reaction conditions. In the synthesis method of sevoflurane, the most commonly used raw material is 1,1,1,3,3,3-hexafluoroisopropanol (hereinafter referred to as hexafluoroisopropanol). Bernad M. Regan et al. reported in US patents US3683092 and US3689571 that hexafluoroisopropanol, polyoxymethylene and anhydrous hydrogen fluoride were reacted in a ratio 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
IPC IPC(8): C07C43/12C07C41/01
Inventor 汪天祥蒋晨郭子维
Owner 福安药业集团重庆博圣制药有限公司
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