Synthesis, structure, immobilization and solid-state NMR of new dppp- and tripod-type chelate linkers

Chelating phosphines incorporating ethoxysilane functions for immobilizations have been synthesized and fully characterized. (EtO)Si(CH2PPh2)3, (EtO)2Si(CH2PPh2)2, and Si(CH2PPh2)4 could be prepared in high yields from cheap starting materials. The ethoxysilanes, as well as a Pd complex thereof have been characterized by X-ray structures, and immobilized on silica. The success of the immobilization was proved by 31P solid-state NMR of the dry materials and of the suspensions. Two representative chelate metal complexes, (EtO)2Si(CH2PPh2)2PdCl2 and (EtO)Si(CH2PPh2)3W(CO)3 have been synthesized, characterized and immobilized.

Graphical abstractThe chelating phosphines (EtO)Si(CH2PPh2)3, (EtO)2Si(CH2PPh2)2, and Si(CH2PPh2)4, and two metal complexes, (EtO)2Si(CH2PPh2)2PdCl2 and (EtO)Si(CH2PPh2)3W(CO)3, have been synthesized in high yields. The ethoxysilane linkers, as well as a Pd complex thereof have been characterized by X-ray structures. All compounds have been successfully immobilized on silica, as proven by 31P solid-state NMR of the dry materials and of the suspensions.Figure optionsDownload full-size imageDownload as PowerPoint slide