A new synthetic approach to substituted unsaturated carboxylic acid derivatives, such as amides, nitriles and esters, has been developed, starting from easily accessible bis-silylated precursors. The key step was based upon the reaction of a bis-silylated diene and a bis- silylated enyne with chlorosulphonyl isocyanate, which afforded mono-silylated amides, easily converted into substituted nitriles and esters.