Abstract
Thermolysis of a 1,3‐dioxa‐2‐phospholane supported by the terphenyl ligand AriPr4 (AriPr4=[C6H3‐2,6‐(C6H3‐2,6‐iPr2)]) at 150 °C gives [AriPr4PO2]2 via loss of ethene. [AriPr4PO2]2 was characterised by X‐ray crystallography and NMR spectroscopy; it contains a 4‐membered P−O−P−O ring and is the isostructural oxygen analogue of Lawesson's and Woollins’ reagents. The dimeric structure of [AriPr4PO2]2 was found to persist in solution through VT NMR spectroscopy and DOSY, supported by DFT calculations. The addition of DMAP to the 1,3‐dioxa‐2‐phospholane facilitates the loss of ethene to give AriPr4(DMAP)PO2 after days at room temperature, with this product also characterised by X‐ray crystallography and NMR spectroscopy. Replacement of the DMAP with pyridine induces ethene loss from the 1,3‐dioxa‐2‐phospholane to provide gram‐scale samples of [AriPr4PO2]2 in 75 % yield in 2 days at only 100 °C.
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