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Preparation method of sevoflurane

A technology of sevoflurane and hexafluoroisopropyl chloromethyl ether is applied in the field of preparation of inhalable anesthetics, and can solve the problems of complex components, harsh reaction conditions, incomplete reaction and the like

Inactive Publication Date: 2014-05-21
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Although a variety of methods for preparing sevoflurane from hexafluoroisopropanol have been disclosed in the prior art, these methods still have many deficiencies, such as not being suitable for industrial production, incomplete reaction, relatively low yield, and raw materials requiring Recycling; harsh reaction conditions such as pressurization and corrosion-resistant equipment; reaction reagents or solvents are not environmentally friendly
In addition, these methods also have the disadvantage of many by-products and complex components.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0035]Add 340g of anhydrous aluminum trichloride and 400g of hexafluoroisopropanol into a 2000mL round-bottomed three-neck flask with mechanical stirring, stir and react for 1 hour under the condition of ice-water bath at 0°C, then add 74g of paraformaldehyde to it , continue the reaction for 1 hour, remove the ice-water bath, and continue the reaction at 25° C. for 24 hours. The HCl gas generated during the reaction is treated with a tail gas absorption device. After the reaction, add 850mL6N hydrochloric acid solution to the slurry-like reaction product, the slurry-like solid dissolves slowly and produces stratification, the lower layer of transparent light yellow hexafluoroisopropyl chloromethyl ether liquid is taken by liquid separation, and distilled, the yield It was 89%, and the GC analysis purity was 99.86%.

Embodiment 2

[0037] Add 200g of hexafluoroisopropyl chloromethyl ether, 300mL of PGE-400 and 100g of potassium fluoride into a 1000mL single-necked round bottom flask equipped with a magnetic stirring and reflux device, and heat to reflux at 80°C for 1 hour in an oil bath . After the reaction, add 150mL of deionized water to dissolve, carry out distillation under normal pressure, collect all the fractions, and obtain 78.31g of sevoflurane crude product, the purity of GC analysis is 61.63%, and the yield is 42.3%. The crude product is obtained after rectification The purity of sevoflurane is 99.97%.

Embodiment 3

[0039] Add 200g of hexafluoroisopropyl chloromethyl ether, 300mL of PGE-400 and 100g of potassium fluoride into a 1000mL single-necked round bottom flask equipped with a magnetic stirring and reflux device, and heat to reflux at 80°C for 3 hours in an oil bath . After the reaction, add 150mL of deionized water to dissolve, carry out distillation under normal pressure, collect all fractions, and obtain 140.7g of sevoflurane crude product, GC analysis purity is 96.89%, yield 76%, the crude product is obtained after rectification The purity of sevoflurane is 99.97%.

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Abstract

The invention discloses a preparation method of sevoflurane. The sevoflurane is prepared from hexafluoroisopropanol, formaldehyde equivalent, aluminum trichloride, a phase transfer catalyst, hindered amine and a metal fluorinating agent as raw materials. The preparation method has the advantages of high yield, high purity, few byproducts and the like, can realize recycling of some raw materials, and is low in cost, easy to control industrially, environment-friendly and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of an inhalable anesthetic, in particular to a preparation method of sevoflurane. Background technique [0002] Sevoflurane, also known as sevoflurane or heptafluoroisopropyl methyl ether, chemical name: fluoromethyl-2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether, is a kind of An inhaled anesthetic drug for the induction and maintenance of general anesthesia. Compared with other inhalational anesthetics, such as fluranes (CF 3 CHFOCHF 2 ), isoflurane (CF 3 CHClOCHF 2 ), enflurane (ClFCHCF 2 OCHF 2 ), sevoflurane has the ideal characteristics of contemporary inhalational anesthetics - rapid loss of consciousness and rapid recovery, so since it was approved for marketing in the United States in 1995, it has attracted great attention. [0003] After decades of technological development, the preparation method of sevoflurane has gone through several stages of development around the different fluorinating...

Claims

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Application Information

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IPC IPC(8): C07C43/12C07C41/22
CPCC07C41/22C07C41/01C07C43/123
Inventor 李义涛郑宝液冯海兵侯琴卿张兵兵
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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