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Pentafluorobenzenesulfonicacid synthesis

6synthesis methods
-

Yield:-

Reaction Conditions:

with water at 100; for 22 h;

Steps:



Scheme 1. (A)Method for Preparing the Precursor benzyl pentafluorobenzenesulfonate (A)2,3,4,5,6-pentafluoro-benzenesulfonyl chloride (3.030 grams, 11.37 millimoles) was added to 8 milliliters H2O. The reaction mixture was heated at100°Centigrade for 22 hours and thereafter concentrated under reduced pressure. Theresulting 2,3,4,5,6-pentafluoro-benzenesulfonic acid was redissolved in 10 mL H2O and silver carbonate (3.125 grams, 11.33 millimoles) was added. After stirring thereaction mixture for 25 hours at room temperature in darkness excess silver carbonatewas filtered off and the filtrate was concentrated under reduced pressure. Theresulting silver salt was dissolved in 9 milliliters dry acetonitrile and benzyl chloride(1.301 grams, 10.28 millimole) was added. Thereafter the mixture was stirred at85°Centigrade in darkness for 17 hours and concentrated under reduced pressure. Theresidue was purified by column chromatography (100 % CEKCl2) yielding I as yellowcrystals (0.350 grams, 10 %).

References:

WO2008/106442,2008,A1 Location in patent:Page/Page column 5; 9; 12-13