A series of five homodimeric polyethylene glycol (PEG) linked homodimers based on the multidrug resistance reversal agent (−)-stipiamide were made and tested for their ability to interact with P-glycoprotein, the protein responsible for multidrug resistance, using ATPase and photoaffinity displacement assays. Key reactions include a new alkoxide-mesylate displacement for the assembly of the PEG linkers and a double Sonogashira coupling ...