The synthesis and characterization of intercalated compound of dodecanesulfornate into hydrated metal, [M($H_2$O)ulcorner](CulcornerHulcorner$SO_3$)$_2$.$xH_2$O (M=Co, Cu) was presented. The compounds shows a layered structure which was determined by powder X-ray diffraction. Thermal behavior of the layered structure was investigated using thermal analysis, and FT-IR spectroscopy by varying the temperature. The increase in layer spacing of the products by increasing the temperature is also checked by X-ray diffraction. We can suggest three kinds of layered structure by varying the temperature, which is accompanied by changing the intercalated dodecanesulfonate from the monolayer to the bilayer structure or changing the tilt angle.