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Process for preparation of trifluoromethanesulfonyl fluoride

A technology of trifluoromethanesulfonyl fluoride and trifluoromethanesulfonyl chloride is applied in the field of manufacture of trifluoromethanesulfonyl fluoride and can solve problems such as cost increase

Inactive Publication Date: 2010-09-22
CENT GLASS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Patent Document 1 discloses a method of making methanesulfonyl chloride (CH 3 SO 2 Cl) A method of producing by electrolytic fluorination, but in this method, a mixed gas of about 20 vol% trifluoromethanesulfonyl fluoride and about 80 vol% hydrogen will be produced by the electrolytic cell, so it is necessary to extract the target from a large amount of hydrogen High-purity purification is carried out by separating the product, and because of this, large-scale electrolysis reaction equipment is required, so there is a problem of cost increase

Method used

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  • Process for preparation of trifluoromethanesulfonyl fluoride

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Embodiment 1

[0049] Feed 103 g (1.78 mol) of 1% aqueous potassium fluoride into a 500 mL pressure-resistant reaction vessel, cool to 5° C. with ice water, and degas under vacuum. Thereto was added trifluoromethanesulfonyl chloride (100 g (0.595 mol)). Close it and slowly raise the temperature, and stir for 4 hours at the inner temperature of the reactor at 40-50°C. At this time, the reactor pressure was 0.94 MPa. The gas in the reactor was circulated in a condenser cooled to -40°C to -20°C, and collected with a trap cooled by liquid nitrogen. 80.3 g of the captured product was obtained, and the generation of trifluoromethanesulfonyl fluoride was confirmed by gas chromatography (GC) analysis, and it was obtained with a purity of 98.9% and a yield of 88% (conversion rate 99%, selectivity 89%). (In addition, in Example 1, "1% aqueous potassium fluoride" means containing 1 mass % of water with respect to 100 mass % of potassium fluoride. Hereafter, it is the same in this specification.)

Embodiment 2

[0051] Feed 103 g (1.78 mol) of 3% aqueous potassium fluoride into a 500 mL pressure-resistant reaction vessel, cool to 5° C. with ice water, and degas under vacuum. Thereto was added trifluoromethanesulfonyl chloride (100 g (0.595 mol)). Airtightly heat up slowly, and stir for 7 hours while the inner temperature of the reactor is 40-50°C. At this time, the reactor pressure was 0.90 MPa. The gas in the reactor was circulated in a condenser cooled to -40°C to -20°C, and collected with a trap cooled by liquid nitrogen. 54.2 g of the captured product was obtained, and the generation of trifluoromethanesulfonyl fluoride was confirmed by gas chromatography (GC) analysis, and it was obtained with a purity of 98.8% and a yield of 81% (conversion rate 99%, selectivity 81%).

[0052] In this way, it can be seen that when the amount of water is reacted in the range of 0.6 mass % to 10.0 mass % with respect to 100 mass % of the metal fluoride, the reaction proceeds well, and the target...

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Abstract

A process for the preparation of trifluoromethanesulfonyl fluoride (CF3SO2F) by reacting trifluoromethanesulfonyl chloride (SF3SO2Cl) with a metal fluoride in the presence of water, characterized in that the amount of water is 0.6 to 10.0mass% based on the metal fluoride (as calculated by taking the amount of the metal fluoride as 100mass%). The process makes it possible to prepare trifluoromethanesulfonyl fluoride by a shortened process, in an enhanced yield, and at an enhanced purity as compared with those of conventional processes.

Description

technical field [0001] The present invention relates to trifluoromethanesulfonyl fluoride (CF) useful as a raw material for the production of intermediates in the fields of organic synthesis, pharmaceuticals, pesticides, and electronic materials, and as a fluorinating reagent. 3 SO 2 F) Manufacturing method. Background technique [0002] As a method for producing fluorine-containing alkanesulfonyl fluoride typified by trifluoromethanesulfonyl fluoride, an electrochemical fluorination method is conventionally known. For example, Patent Document 1 discloses a method of making methanesulfonyl chloride (CH 3 SO 2 Cl) A method of producing by electrolytic fluorination, but in this method, a mixed gas of about 20 vol% trifluoromethanesulfonyl fluoride and about 80 vol% hydrogen will be produced by the electrolytic cell, so it is necessary to extract the target from a large amount of hydrogen There is a problem of high-purity purification by separating the product and requiring...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/08C07C309/80
CPCC07C303/22
Inventor 坂井繁则森中孝敬南明勉久米孝司
Owner CENT GLASS CO LTD
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