ChemicalBook CAS DataBase List Trifluoromethanesulfonic acid

Trifluoromethanesulfonic acid synthesis

14synthesis methods

Product Name:Trifluoromethanesulfonic acid
CAS Number:1493-13-6
Molecular formula:CHF3O3S
Molecular Weight:150.08

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Yield:1493-13-6 167.5 g

Reaction Conditions:

Stage #1: Bromotrifluoromethanewith iodine;zinc in tetrahydrofuran at 40 - 50; for 5 h;Inert atmosphere;
Stage #2: with sulfur trioxide in tetrahydrofuran; for 2 h;Inert atmosphere;

Steps:

1

Under nitrogen protection, 212 g of zinc powder in 1 L of tetrahydrofuran was passed 100 g of trifluorobromomethane liquid, Then add a catalytic amount of elemental iodine, slowly heated to 40 ° C, After the response should be made, Then slowly pass 300g of trifluorobromomethane, control temperature does not exceed 50°C. After stirring for 5h, Slowly add 260g of sulfur trioxide solid, stir the reaction after the completion of feeding 2h. The reaction solution was neutralized with 30% aqueous sodium hydroxide solution,When precipitation no longer occurs, the solid is filtered off and the filtrate evaporated to dryness to give the sodium triflate as a solid. The sodium salt and 240g of concentrated sulfuric acid were mixed and stirred at 100 ° C for 5h, the distillation was trifluoromethanesulfonic acid 167.5g. (Content: 99.97%; F-: 7 ppm; Cl-: 0 ppm; SO42-: 8 ppm)

References:

CN104725283,2016,B Location in patent:Paragraph 0030; 0031