Defluorinations of fluoroformal and fluoroether were carried out with SbF3 and a catalytic amount of Br2 in SO2Cl2 at room temperature. Bis (2-chloro-2, 2-difluoroethyl) difluoroformal and 2-chloro-1, 1, 2-trifluoroethyl methyl ether were converted to bis (2-chloro-2, 2- difluoroethyl) carbonate and methyl chlorofluoroacetate, respectively.