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Method for preparing sevoflurane

A fluoromethyl and fluoride technology, applied in the field of preparation of sevoflurane, can solve the problems of low yield of sevoflurane, difficult purification and the like, and achieves low production cost, high conversion rate of raw materials, significant social and economic benefits Effect

Active Publication Date: 2011-09-28
JIANGSU HENGRUI MEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

WO2006055748 reported the fluorination reaction of chloromethyl-2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether catalyzed by quaternary ammonium salt or quaternary phosphonium salt as phase transfer catalyst, in the reaction system Usually 5%-30% of chloromethyl-2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether cannot be converted, and the yield of sevoflurane is low and difficult to purify

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] In a 250mL three-necked flask, add 100 grams of chloromethyl-2,2,2-trifluoro-1-(trifluoromethyl) ethyl ether (made according to document USP3683092), 328 grams of sulfolane, 16 grams of water, 20 gram pentaerythritol and 70 grams of potassium fluoride, heated to 100 ° C, and stirred at 100 ° C for 10 hours, after analysis, it contained 91.8% of sevoflurane, and the conversion rate was greater than 99.0%. The rate is 73.4%.

Embodiment 2

[0013] In a 100mL three-necked flask, add 20.0 grams of chloromethyl-2,2,2-trifluoro-1-(trifluoromethyl) ethyl ether, 65.5 grams of sulfolane, 3.2 grams of water, 8.0 grams of 1,2,3- Glycerol and 14.0 g of potassium fluoride are heated to 100° C. and stirred at 100° C. for 8-9 hours. After analysis, the mixture contains 91.6 percent of sevoflurane, and the conversion rate is greater than 99.0 percent. After the reaction was completed, 12.5 grams of product were obtained by distillation with a purity of 97.6% and a yield of 67.5%.

Embodiment 3

[0015] In a 100mL three-necked flask, add 20.0 grams of chloromethyl-2,2,2-trifluoro-1-(trifluoromethyl) ethyl ether, 65.5 grams of sulfolane, 3.2 grams of water, 3.7 grams of erythritol and 14.0 grams of Potassium fluoride was heated up to 100°C and stirred at 100°C for 6 hours. After analysis, it contained 84.8% of sevoflurane, and the conversion rate was greater than 99.0%. After the reaction was completed, 13.0 grams of product were obtained by distillation with a purity of 92.2% and a yield of 70.2%.

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PUM

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Abstract

The invention relates to a method for preparing sevoflurane (i.e. methyl fluoride-2,2,2-trifluoro-1- (trifluoromethyl) ethylether), which comprises the steps of: reacting chloromethyl-2,2,2-trifluoro-1- (trifluoromethyl) ethylether) with fluoride. The method has the advantages of simple operation, low cost, high yield and easiness in recycling the solvent, and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to a preparation method of fluoride, in particular to a preparation method of sevoflurane. Background technique [0002] Sevoflurane (i.e., fluoromethyl-2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether) is an inhalational anesthetic, and in many sevoflurane preparation methods, chloromethyl - The fluorination reaction of 2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether is a key step in the preparation of sevoflurane. US3,683,092 reports that chloromethyl-2,2,2-trifluoro-1-(trifluoromethyl)ethyl ether reacts with potassium fluoride in sulfolane solvent to generate sevoflurane. The process of the fluorination reaction in this method is slow and the conversion rate is low, and the product is difficult to purify. US6,100,434 reported that chloromethyl-2,2,2-trifluoro-1-(trifluoromethyl) ethyl ether reacted with fluorinated reagent (such as KF, NaF) in solvent PEG-400 to prepare sevoflurane , and achieved better results. EP0901...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/12C07C41/22
Inventor 张富尧神小明孙飘扬
Owner JIANGSU HENGRUI MEDICINE CO LTD
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