Direct Electrochemical Synthesis and Crystal Structure of Copper(I) Complex with 2′‐hydroxy‐5′‐methyl‐acetophenone and Triphenylphosphine Ligands

Abstract

A new complex of Cu with 2′‐hydroxy‐5′‐methyl‐acetophenone (HMAP) and triphenylphosphine (PPh₃) was prepared by the electrochemical oxidation of Cu in acetonitrile solutions. The final product, (MAP)Cu(PPh₃)₂, was crystallized from bulk solution and characterized by microanalysis, IR, Raman, ¹H NMR together with x‐ray crystallographic determinations. The results showed that the complex was a chelate structure in which Cu(I) ion was coordinated with two oxygen atoms of the deprotonated ligand of MAP anion to form a six member ring, and two PPh₃ molecules participated in the coordination. The parameters of the complex were monoclinic, space group of P2₁/n, a=9.048(2) Å, b=26.405(6) Å, c=15.606(4) Å, β=95.990(5)°, Z=4, R=0.057 for 8428 unique reflections. The details of synthesis, reaction mechanism on the electrode and the effect of PPh₃ on the coordinating processes are discussed.

Keywords:

• Copper
• crystal structure
• direct electrochemical synthesis

Acknowledgments

This work was partially supported by the key organic synthesis laboratory of Jiangsu Province of Suzhou University.