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A series of asymmetric phenylacetylene tridendrons is prepared by coupling polar monodendrons having t-butyl esters on their periphery with a non-polar monodendron having t-butyl groups on its periphery. Subsequent conversion of the t-butyl esters to carboxylic acids by thermolysis gives amphiphilic dendrimers having polar domains of various size. The characterization and solution phase behav or of these structures is discussed.