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ChemicalBook CAS DataBase List Trifluoromethanesulfonyl bromide

Trifluoromethanesulfonyl bromide synthesis

5synthesis methods
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Yield:15458-53-4 68.8 kg

Reaction Conditions:

with chlorine;sodium bromide in water at 0;Large scale;

Steps:

1 Example 1

In a 2000L steel reaction kettle, add 300kg of water, 200kg of acetonitrile, 150kg of trisodium phosphate, 25kg of sodium hydroxide and 85kg of sodium dithionite, raise the temperature to 55°C, and feed 60kg of bromotrifluoromethane. After 3 hours of reaction, the reaction is complete. Add ethyl acetate for extraction three times, combine the organic phases and then desolventize to obtain sodium trifluoromethylsulfinate, add 200kg of water and 60kg of sodium bromide, cool down to 0°C, and introduce chlorine gas under stirring, chlorine gas and perfluoroalkylsulfinate The molar ratio of sodium sulfonate is 0.95:1. After the reaction is completed, the liquid is separated, and the lower organic phase is washed with 1wt% sodium bisulfite aqueous solution. After washing three times, the lower product phase is released to the rectification tower, and the 35°C fraction at the top of the tower is collected. , to obtain 68.8kg of product trifluoromethylsulfonyl bromide, with a content of 99.7%, and a yield of 80%.

References:

CN115521232,2022,A Location in patent:Paragraph 0040-0043

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