The basic problem of a homogeneous catalytic process is the separation of products from catalytic reaction system. Two main important developments, to immobilize the solid complex catalyst on the solid support and to use the two-phase (aqueous-organic solvent) catalysis, have achieved to solve this problem. However, some difficulties, such as the continuous loss of the catalyst and lower aqueous solubility of the ubstrate, still remain as before[1,2]. Recently, a complex catalyst of nonmetal selenium with triethylamine in the presence of CO, which possesses the reaction process phase transfer property, has been developed[3～7]. This catalytic system provides both advantages from homogeneous catalysis and heterogeneous catalysis, resulting in simple and complete separation of the product from the catalytic system. It differs from the two-phase catalysis, in our catalytic system no water was used as solvent, and the catalytic system is effective in selective oxidative-reductive carbonylation with nitroaromatic compounds and alkylamine as reagents at the same time[5～7]. Monuron is a kind of herbicide. The methods for its industrial synthesis use mainly the phosgene, but the phosgene has high toxicity and produces a lot of corrosive contaminants[8,9]. Our study is extended to the selective oxidative-reductive carbonylation of p-ClC6H4NO2 and 33%HN(CH3)2-67%H2O in one-pot reaction to give monuron.