1,3-bis[5-(4-ethyoxycarbonyl)phenyl-10,15,20-tri(4-chlorophenyl)porphyrin]-5-fluorouracil(A),1-[5-(4-ethoxycarbonyl)phenyl-10,15,20-tri(4-chlorophenyl)porphyrin]-5-fluorouracil(B) are synthesized.Their structures are characterized by UV-Vis,IR,1HNMR and MS.The synthesis and separation conditions of the target compounds are studied.The results show that the yield is higher when DMF is used as the solvent at 115 ℃ for 11 h.The products are separated via column chroma to graphy with silica gel(200-300) separation is more satisfactory as the eluent when the column is 3 cm in diameter and 12 cm in height.