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The fabrication of compartmented micellar systems is an exciting new area of research in the field of polymer self-assembly. Multicompartment micelles composed of a water-soluble shell and a segregated hydrophobic core can be obtained via direct aqueous self-assembly of preformed polymeric amphiphiles possessing one hydrophilic segment and two incompatible hydrophobic segments (e.g. hydrocarbon and fluorocarbon blocks). Such macromolecular building-blocks were prepared in the present work principally via reversible addition-fragmentation transfer polymerization (RAFT). Polysoaps or triblock macrosurfactants can be synthesized in high yields by RAFT under relatively straightforward experimental conditions.