Inclusion compounds (intercalates) of fluorinated graphite matrix with chloroform (C2FxBrz·yCHCl3, x=0.49, 0.69, 0.87, 0.92, z=0.01) were synthesized by guest substitution from acetonitrile to chloroform. The kinetics of the thermal decomposition (the 1st stage of filling → the 2nd stage of filling) was studied under isothermal conditions at 286–311 K. The relationship between the structure of matrices intercalates with thermal properties and kinetic parameters of inclusion compounds is discussed.