A modified poly(ethylene glycol) (PEG) has been developed for the soluble polymer-supported combinatorial synthesis of novel thiourea derivatives. Dihydroxy-PEG with an average MW of 4000 was used as soluble polymer supports. a benzoyl residue as spacer, and 4-oxybenzoyl chloride group as the moiety with the reactive functionality. Representative thiourea derivatives were obtained in moderate to high yields with excellent purity from these modified PEG-bound products by cleavage with 6% ammonium water. In each step of the sequence, the PEG-bound products were precipitated in cold Et2O and the excessive reagents and by-products were removed by simple filtration. The progress of reaction, purities of the isolation and the configuration of the PEG-bound products, were easily monitored by TLC, IR and H-1 NMR (C) 2002 Published by Elsevier Science B.V.