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Tris(β-diketimine) cyclophanes are an important ligand class for investigating cooperative multimetallic interactions of bioinorganic clusters. Discussed herein are the synthetic factors governing access to tris(β-diketimine) cyclophanes versus tripodal tri-β-aminoenones. Cyclophanes bearing Me, Et, and MeO cap substituents and β-Me, Et, or Ph arm substituents are obtained, and a modified condensation method produced α-Me β-Me cyclophane. These operationally simple procedures produce the ligands in gram quantities and in 22-94% yields.

Synthetic Factors Governing Access to Tris(β-diketimine) Cyclophanes versus Tripodal Tri-β-aminoenones