This invention relates to a series of fluoroalkylsilane compounds of formula I. ##STR1## These compounds are silylation reagents which enhance the solubility of the silylated products in fluorocarbon solvents for preferred use in fluorous phase synthesis. Use of these compounds protects fragile hydrogen groups and also provides for the straightforward separation of the ultimate reaction products though fluorous phase extraction. This invention also relates to a two-step process for making compounds of formula I. The process comprises reacting an alkyldialkoxysilane with a perfluoroalkyl-substituted silane to produce a perfluoroalkyl-substituted dialkylsiloxyalkylsilane intermediate; and reacting the intermediate with halogen.