The synthesis of small-ring lactams I [R1 = CH2Ph, n-Bu, n-C11H23, CH2CCH; R2 = n-Bu, (CH2)nCO2H; R3 = Me, 4-BrC6H4, Ph, CO2H; n = 10, 5, 2], via the condensation of ω-keto acids R3CO(CH2)mCH2CO2H (m = 1, 2), isocyanides R2NC and amines R1NH2 is reported. This process is shown to proceed well in a combinatorial fashion, by immobilization of the isocyanide component on Wang resin. The product is then released from the support on treatment with 10% TFA/CH2Cl2.