Abstract A fundamentally new preparation of internal and terminal gem-bis-(difluoramino) alkanes has been demonstrated by the direct fluorination of corresponding gem- bisacetamides, specifically, 1, 1-bisacetamidocyclohexane and 1, 1-bisacetamidopropane, leading to 1, 1-bis (difluoramino) cyclohexane and 1, 1-bis (difluoramino)-propane, respectively.