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666836-33-5

Methanesulfonic acid, 1,1,1-trifluoro-, 2,2,2-trifluoro-1-[4-(trifluoromethyl)phenyl]ethyl ester synthesis

2synthesis methods
-

Yield:666836-33-5 78%

Reaction Conditions:

with 2,6-dimethylpyridine in dichloromethane at -20 - 10; for 3 h;Inert atmosphere;

Steps:

48.2 Step 2: Synthesis of 2,2,2-trifluoro-1-(4-(trifluoromethyl)phenyl) ethyl trifluoromethanesulfonate

Under the protection of nitrogen, 2,2,2-trifluoro-1-(4-(trifluoromethyl)phenyl)ethanol (918mg, 3.76mmol) was dissolved in DCM (10mL), and at -20, add 2 , 6-lutidine (0.90mL, 8.00mmol) and Tf2O (0.95mL, 5.60mmol), then stirred at 10°C for 3h. To the reaction solution was added saturated NaHCO3 solution (80mL) to quench the reaction, DCM (100mL) was extracted, the organic phase was washed with HCl solution (50mL×2, 1M), dried with anhydrous Na2SO4, and concentrated under reduced pressure to obtain a yellow oil (1.1 g, 78.0%).

References:

CN113072546,2021,A Location in patent:Paragraph 0968; 0972-0973