The preparation of a fluorous super Bronsted acid catalyst, 4-(1H,1H-perfluorotetradecanoxy)-2,3,5,6-tetrafluorophenylbis(trifluoromethanesulfonyl)methane (3d), is described. The fluorouscatalyst 3d can be recycled by using liquid/solid phase separation without fluorous solvents. A perfluorocarbon solvent is not essential for fluorous biphasic catalysis.