Methyl N-phenyl carbamate (MPC) is synthesized from aniline and dimethyl carbonate using Pb compounds as catalysts. Using Pb(OAc) 2·Pb(OH) 2 as a catalyst, 97% of aniline present is converted into MPC with 95% selectivity at 453 K in 1 h. In the case of PbO catalyst, an induction period was observed and it disappeared when the catalyst was pretreated with dimethyl carbonate or methanol. The effects of the reaction variables are examined in the reaction using Pb(OAc) 2·Pb(OH) 2 as the catalyst and the reaction mechanism is discussed.