The synthesis of amphiphilic carbosilane dendrimers that contain perfluoroalkyl and hydroxy groups at terminal positions is explored in this work. Zeroth- and first-generation hydroxyallyl dendrimers were reacted with a heptadecafluorodecane hydrosilane to produce the new first- and second-generation derivatives in 58% and 55% yields, respectively. The reaction of a zeroth-generation carbosilane dendrimer with four terminal ester groups with 1,1,2-trifluorobut-1-enyl-4-magnesium bromide gave another type of the first-generation polyfluorinated amphiphilic derivative under mild conditions in 58% yield. Their compositions were confirmed by NMR and IR spectroscopy as well as mass spectrometry and elemental analyses. The thermal stabilities were evaluated by differential scanning calorimetry and thermogravimetric analysis. Polyfluoroalkylation increased the thermal stability of the amphiphilic carbosilane dendrimers relative to their nonfluorinated precursors. IR results showed that the amphiphatic dendrimers were useful for solubilizing pentoxyfylline (antibiotic) in perfluoro solvents (perfluorobenzene, perfluorodecalin, and perfluorooctyl bromide).