Formula _{CF 3 (CF 2) n (} CH 2 CF 2) a (CF 2 CF 2) b CH 2 CH = CH 2 [I] (n: 0~5, a: 1 or 2, b: 0 to 3 polyfluoroalkyl allyl compounds represented by). The polyfluoroalkyl allyl compounds have the general formula _{CF 3 (CF 2) n (} CH 2 CF 2) a (CF 2 CF 2) b CH 2 CHICH 2 OCOR' [II] (n, a, b: the definitions and the same, R': carboxylic acid allyl adduct represented by the alkyl group) having 1 to 3 carbon atoms, is prepared by reacting a transition metal. In this manufacturing method, without the use of high metal reagent environmental load, it is possible to remove free iodine derived from the raw material compounds prior to the hydrosilylation reaction and handling properties also show good fluorine-containing alkyl silane compound providing a polyfluoroalkyl allyl compounds used as synthetic intermediates.